CN107177820B - Method high speed continuous type vacuum vapor deposition lithium equipment and realize substrate vapor deposition lithium using it - Google Patents
Method high speed continuous type vacuum vapor deposition lithium equipment and realize substrate vapor deposition lithium using it Download PDFInfo
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- CN107177820B CN107177820B CN201710438908.4A CN201710438908A CN107177820B CN 107177820 B CN107177820 B CN 107177820B CN 201710438908 A CN201710438908 A CN 201710438908A CN 107177820 B CN107177820 B CN 107177820B
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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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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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
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/562—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates
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Abstract
Method high speed continuous type vacuum vapor deposition lithium equipment and it is utilized to realize substrate vapor deposition lithium, it is related to a kind of substrate vapor deposition lithium equipment and the method using its realization substrate vapor deposition lithium.Low to the utilization rate of lithium metal the invention aims to solve existing substrate vapor deposition lithium equipment, evaporation thickness is≤1 μm, pollution range big problem when vapor deposition.The continuous type vacuum vapor deposition lithium equipment of high speed includes body fuselage, cavity dam, unwinding system, substrate heater, home roll, chill roll, winding system, crucible, crucible fixed frame, crucible heater, insulating layer, crucible lifting-transverse shifting platform, unreels transition roller, heating transition roller, cooling transition roller, epicoele vacuum valve, cavity of resorption vacuum valve and charging visual windows；Method: guarantee to adjust at any time between 1 μm~100 μm of evaporation thickness range, lithium metal optimum rate of utilization can reach 90% or more.Present invention is mainly used for substrates, and lithium is deposited.
Description
Technical field
The present invention relates to a kind of substrate vapor deposition lithium equipment and the methods for realizing substrate vapor deposition lithium using it.
Background technique
Elemental lithium material property are as follows: lithium is easy to burn with the chemical combination such as oxygen, nitrogen, sulphur, chance water, and storage condition strictly waits spies
Point, so can only carry out being heated into gaseous state vapor deposition to lithium metal in high vacuum.Existing large scale equipment be AM aluminum metallization, nickel,
The materials such as zinc, and the utilization rate of small-sized evaporation metal lithium equipment only has between 2%~10%, evaporation thickness is≤1 μm, if
Evaporation thickness increases, and is deposited in chamber when uniformity not can guarantee and be deposited and is full of lithium steam, and pollution range is big equal scarce when vapor deposition
Point.
Summary of the invention
It is low to the utilization rate of lithium metal the invention aims to solve existing substrate vapor deposition lithium equipment, evaporation thickness is≤
1 μm, pollution range big problem when vapor deposition, and the continuous type vacuum vapor deposition lithium equipment of high speed is provided and realizes substrate using its
The method that lithium is deposited.
The continuous type vacuum vapor deposition lithium equipment of high speed, it includes that body fuselage, cavity dam, unwinding system, substrate add
Hot device, home roll, chill roll, winding system, crucible, crucible fixed frame, crucible heater, insulating layer, crucible lifting-transverse shifting platform,
Unreel transition roller, heating transition roller, cooling transition roller, epicoele vacuum valve, cavity of resorption vacuum valve and charging visual windows；
The continuous type vacuum vapor deposition lithium equipment of high speed is separated into upper cavity and cavity of resorption by cavity dam and body fuselage
Body, the unwinding system, substrate heater, chill roll and winding system setting are in the continuous type vacuum vapor deposition lithium equipment of high speed
Upper cavity in, the transition roller that unreels is arranged between unwinding system and substrate heater, and the heating transition roller, which is arranged, to exist
Between home roll and substrate heater, the cooling transition roller is arranged between home roll and chill roll；The crucible, crucible are fixed
Frame, crucible heater, insulating layer and crucible lifting-transverse shifting platform are arranged under the continuous type vacuum vapor deposition lithium equipment of high speed
In cavity, the crucible fixed frame is fixedly connected with body fuselage inner wall, and the insulating layer is arranged in crucible lifting-transverse shifting platform
On, the crucible is carried on crucible fixed frame, and when lithium is deposited, the crucible is placed in crucible heater, and the crucible
Top it is in curved surface parallel with home roll；Using insulating layer cladding crucible heater for keeping the temperature；On epicoele body sidewall in setting
Cavity of resorption vacuum valve is arranged in lower chamber side wall upper part in chamber vacuum valve, and charging visual windows are arranged in lower chamber top side wall；
The home roll passes through cavity dam, and a part is in upper cavity, and another part is in lower chamber, and home roll and cavity dam
Distance be 5mm~10mm；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes coating detection system, is examined using coating detection system
Survey chill roll and cooling transition roller and between substrate surface coating thickness；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes pumped vacuum systems, using pumped vacuum systems to high speed
The upper cavity and lower chamber of continuous type vacuum vapor deposition lithium equipment carry out vacuumize process；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes PLC control system, is controlled using PLC control system
The continuous type vacuum vapor deposition lithium equipment running of high speed；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes crucible cooling system, the crucible cooling system packet
Containing cooling oil, crucible is silicon-controlled and crucible cooler, and the side wall of the crucible fixed frame is hollow structure, and cooling oil is loaded in earthenware
In the hollow structure of crucible fixed frame side wall, it is cold that oil carried out to crucible using cooling oil, using crucible is silicon-controlled and crucible cooler
Circulating cooling is carried out to cooling oil.
The method for realizing substrate vapor deposition lithium using the continuous type vacuum vapor deposition lithium equipment of high speed, specifically according to the following steps
It completes:
One, the preparation stage: upper cavity is closed after 1., by substrate being worn in the continuous type vacuum vapor deposition lithium equipment of high speed
And lower chamber, it 2., by lithium metal along charging visual windows is added in crucible, then crucible is moved in crucible heater, and
Crucible is put consistent with home roll direction, adjusts crucible lifting-transverse shifting platform, make crucible and home roll surface substrate distance 5mm~
3., to the continuous type vacuum vapor deposition lithium equipment of high speed 20mm is sealed；
Two, it vacuumizes: the upper cavity of the continuous type vacuum vapor deposition lithium equipment of high speed being vacuumized, until the vacuum of upper cavity
Degree is 6.5 × 10-2Pa~7 × 10-2Until Pa, while the lower chamber of the continuous type vacuum vapor deposition lithium equipment of high speed is taken out true
Sky, until the vacuum degree of lower chambers is 7 × 10-3Pa~7 × 10-4Until Pa；
Three, it is deposited: starting crucible heater, and lithium metal temperature in real-time detection crucible, when lithium metal temperature in crucible
When reaching 350 DEG C, starting unwinding system, substrate heater and winding system, the continuous type vacuum vapor deposition lithium of adjustment high speed are set
Standby operating parameter until substrate surface lithium layer thickness reaches actual requirement, and guarantees high speed under the conditions of current operating parameter
Continuous type vacuum vapor deposition lithium equipment carries out normal；
Four, cooling pressure release: after completing substrate vapor deposition lithium, closing crucible heater, unwinding system, substrate heater and winding
System adjusts crucible lifting-transverse shifting platform, crucible is moved on crucible fixed frame, and crucible is cooled to 40 using oil cold mode
~50 DEG C, the vacuum pressure of upper cavity and lower chamber is released at this time；
Five, it takes substrate: opening the upper cavity and lower chamber of the continuous type vacuum vapor deposition lithium equipment of high speed, take out surface and steam
Plate lithium substrate.
The invention has the advantages that one, setting will the continuous type vacuum vapor deposition lithium equipment of high speed by cavity dam and body fuselage
It is separated into upper cavity and lower chamber, the vacuum degree of upper cavity is 6.5 when preventing lithium steam when vapor deposition from polluting to substrate, and lithium is deposited
×10-2Pa~7 × 10-2Pa, the vacuum degree of lower chambers are 7 × 10-3Pa~7 × 10-4Pa；The high vacuum values of lower vapor deposition chamber can mention
The adhesive force of high lithium and substrate, and lithium is inhibited to provide advantage to epicoele pollution；Two, crucible is deposited and substrate distance is
5mm~20mm spacing, and be deposited crucible put it is consistent with home roll direction, guarantee 1 μm~100 μm of evaporation thickness range between can
It adjusts at any time, 1 μm of tolerance+, the effective utilization rate for improving lithium metal, lithium metal optimum rate of utilization can reach 90% or more, section
Cost-saving, and homogeneity reaches ± 95%；Three, the continuous type vacuum vapor deposition lithium equipment of present invention high speed has explosion-proof, sealing
Property good, anti-high pressure, high-temperature heating, cooling down and automatic detection steam thickness of coating function, be large-scale continuous safety in production
The advantageous guarantee provided.
Detailed description of the invention
Fig. 1 is the continuous type vacuum vapor deposition lithium device structure schematic diagram of high speed described in specific embodiment one.
Specific embodiment
Specific embodiment 1: present embodiment is the continuous type vacuum vapor deposition lithium equipment of high speed, it is wrapped in conjunction with Fig. 1
Include body fuselage 1, cavity dam 2, unwinding system 3, substrate heater 4, home roll 5, chill roll 6, winding system 7, crucible 8, earthenware
Crucible fixed frame 9, crucible heater 10, insulating layer 11, crucible lifting-transverse shifting platform 12, unreel transition roller 13, heating transition roller 14,
Cooling transition roller 15, epicoele vacuum valve 16, cavity of resorption vacuum valve 17 and charging visual windows 18；
The continuous type vacuum vapor deposition lithium equipment of high speed is separated into upper cavity under by cavity dam 2 and body fuselage 1
Cavity, the unwinding system 3, substrate heater 4, chill roll 6 and winding system 7 are arranged in the continuous type vacuum vapor deposition of high speed
In the upper cavity of lithium equipment, the transition roller 13 that unreels is arranged between unwinding system 3 and substrate heater 4, described heated
It crosses roller 14 to be arranged between home roll 5 and substrate heater 4, the cooling transition roller 15 is arranged between home roll 5 and chill roll 6；
The crucible 8, crucible fixed frame 9, crucible heater 10, insulating layer 11 and the setting of crucible lifting-transverse shifting platform 12 are continuous in high speed
In the lower chamber of type vacuum vapor deposition lithium equipment, the crucible fixed frame 9 is fixedly connected with 1 inner wall of body fuselage, the guarantor
Warm layer 11 is arranged on crucible lifting-transverse shifting platform 12, coats crucible heater 10 using insulating layer 11 and is used to keep the temperature, the earthenware
Crucible 8 is carried on crucible fixed frame 9, and when lithium is deposited, the crucible 8 is placed in crucible heater 10, and the top of the crucible 8
Portion is in curved surface parallel with home roll 5；Epicoele vacuum valve 16 is set on epicoele body sidewall, cavity of resorption is set in lower chamber side wall upper part
Charging visual windows 18 are arranged in lower chamber top side wall in vacuum valve 17；The home roll 5 is at cavity dam 2, a part
In upper cavity, another part is in lower chamber, and home roll 5 is 5mm~10mm at a distance from cavity dam 2；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes coating detection system, is examined using coating detection system
Survey chill roll 6 and cooling transition roller 15 and between substrate surface coating thickness；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes pumped vacuum systems, using pumped vacuum systems to high speed
The upper cavity and lower chamber of continuous type vacuum vapor deposition lithium equipment carry out vacuumize process；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes PLC control system, is controlled using PLC control system
The continuous type vacuum vapor deposition lithium equipment running of high speed；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes crucible cooling system, the crucible cooling system packet
Containing cooling oil, crucible is silicon-controlled and crucible cooler, and the side wall of the crucible fixed frame 9 is hollow structure, and cooling oil is loaded in
In the hollow structure of 9 side wall of crucible fixed frame, it is cold that oil carried out to crucible 8 using cooling oil, using crucible is silicon-controlled and crucible is cold
But machine carries out circulating cooling to cooling oil.
Fig. 1 is the continuous type vacuum vapor deposition lithium device structure schematic diagram of high speed described in present embodiment one, 1 expression in figure
Body fuselage, 2 indicate cavity dam, and 3 indicate unwinding system, and 4 indicate substrate heating, and 5 indicate home roll, and 6 indicate chill roll, 7 tables
Show winding system, 8 indicate crucible, and 9 indicate crucible fixed frame, and 10 indicate crucible heater, and 11 indicate insulating layer, and 12 indicate crucible
Lifting-transverse shifting platform, 13 indicate to unreel transition roller, and 14 indicate heating transition roller, and 15 indicate cooling transition roller, and 16 indicate that epicoele is true
Empty valve, 17 indicate cavity of resorption vacuum valve, and 18 indicate charging visual windows.
Coating detection system described in present embodiment is X-ray thickness gauge.
Pumped vacuum systems described in present embodiment includes oil-sealed rotary pump, Roots vaccum pump and molecular pump.
PLC control system described in present embodiment includes feeding and threading process, each parameter setting process, automatic running-
Substrate pre-add thermal flow process, automatic running-home roll heating procedure, automatic running-lithium material heating evaporation process, automatic running-substrate
Cooling process, automatic fortune after conveying process, automatic running-continuous evaporating-plating thickness measuring and thickness control process, automatic running-vapor deposition
Row-tension force process, automatic running-tension force process, automatic running-winding uniformity process, automatic running-winding are whole
Neat degree process, automatic running-flattening process and automatic running-coiled strip surplus detection and shutdown process.
Continuous principle of the type vacuum vapor deposition lithium equipment as other vacuum coating equipments of high speed, requires in high vacuum
Good evaporation effect is obtained under state, the continuous type vacuum vapor deposition lithium equipment of high speed is to connect due to its special working principle
Continuous vapor deposition, often vacuum chamber is more much bigger than common coating machine spatial volume, needs with 2 opposing spaced apart of cavity dam to be coiling chamber
(upper cavity) and vaporization chamber (lower chamber) two major parts, evaporant will not just be polluted into coiling chamber, keep the phase of coiling chamber
To cleaning, since home roll 5 is 5mm~10mm at a distance from cavity dam 2, base material thickness is micron order, therefore substrate passes through master
Crack disengaging coiling chamber and vaporization chamber between roller 5 and cavity dam 2.Coiling chamber is due to there is the presence of basement membrane, and in continuous work
In the process, basement membrane itself and interlayer discharge quantity are very big, and the discharge quantity of vaporization chamber is relatively small.Coiling chamber and vaporization chamber are two phases
To independent space, and the vacuum pump of the two configuration is variant；The main pumping pump configuration of coiling chamber is the opposite lesser vacuum of pumping speed
Pump, the main pumping pump configuration of vaporization chamber is the opposite very big vacuum pump of pumping speed, although being connection between two chamber bodies, due to master
Roller 5 is 5mm~10mm at a distance from cavity dam 2, and there are crack effect, the vacuum degree difference between two rooms is obvious
's；Since evaporation material is that gas procedure exists in vaporization chamber, need to work under higher vacuum degree condition, and coiling chamber
Interior, evaporation material has been solidified as solid, is not needing condition of high vacuum degree to maintain, it is only necessary to compared with rough vacuum.Furthermore it winds
Vacuum pump is separately separately configured in room and vaporization chamber, also there is the considerations of save the cost.If necessary to which coiling chamber is also maintained at Gao Zhen
The pump of reciprocal of duty cycle, configuration just needs bigger pumping speed, and cost performance is not high.
Specific embodiment 2: the difference of present embodiment and specific embodiment one is: described to unreel in conjunction with Fig. 1
System includes let off roll, deviation-rectifying system, transition roller system, substrate evaporation rate control system, tension control system and flattening system
System.Other are same as the specific embodiment one.
Specific embodiment 3: one of present embodiment and specific embodiment one or two difference are: institute in conjunction with Fig. 1
State winding system include wind-up roll, mechanical expansion shaft, AC driven motor, frequency-variable controller, SKF bearing, magnet fluid sealing and on
Expect turntable.Other are the same as one or two specific embodiments.
Specific embodiment 4: one of present embodiment and specific embodiment one to three difference are: institute in conjunction with Fig. 1
It is silicon-controlled to state setting temperature transmitter and home roll on home roll 5.Other are identical as specific embodiment one to three.
Specific embodiment 5: one of present embodiment and specific embodiment one to four difference are: institute in conjunction with Fig. 1
It states chill roll 6 and connects silicon-controlled and cooler.Other are identical as specific embodiment one to four.
Specific embodiment 6: one of present embodiment and specific embodiment one to five difference are: institute in conjunction with Fig. 1
The material for stating body fuselage 1 is stainless steel, thickness 50mm.Other are identical as specific embodiment one to five.
Specific embodiment 7: one of present embodiment and specific embodiment one to six difference are: institute in conjunction with Fig. 1
Crucible 8 is stated as semicircle or rectangle, and the diameter ratio of the width of the crucible 8 and home roll 5 is 1:(3~10).Other and tool
Body embodiment one to six is identical.
Specific embodiment 8: present embodiment is continuous using high speed described in specific embodiment one to seven in conjunction with Fig. 1
The method that type vacuum vapor deposition lithium equipment realizes substrate vapor deposition lithium, is specifically realized by the following steps:
One, the preparation stage: upper cavity is closed after 1., by substrate being worn in the continuous type vacuum vapor deposition lithium equipment of high speed
And lower chamber, it 2., by lithium metal along charging visual windows 18 is added in crucible 8, crucible 8 is then moved to crucible heater 10
On, and crucible 8 is put consistent with home roll direction, adjusts crucible lifting-transverse shifting platform 12, makes crucible 8 and 5 surface substrate of home roll
Distance is 5mm~20mm, 3., to the continuous type vacuum vapor deposition lithium equipment of high speed is sealed；
Two, it vacuumizes: the upper cavity of the continuous type vacuum vapor deposition lithium equipment of high speed being vacuumized, until the vacuum of upper cavity
Degree is 6.5 × 10-2Pa~7 × 10-2Until Pa, while the lower chamber of the continuous type vacuum vapor deposition lithium equipment of high speed is taken out true
Sky, until the vacuum degree of lower chambers is 7 × 10-3Pa~7 × 10-4Until Pa；
Three, it is deposited: starting crucible heater 10, and lithium metal temperature in real-time detection crucible 8, when lithium metal in crucible 8
When temperature reaches 350 DEG C, starting unwinding system 3, substrate heater 4 and winding system 7, the continuous take-up type vacuum of adjustment high speed steam
Lithium equipment operating parameter is plated, is protected until substrate surface lithium layer thickness reaches actual requirement, and under the conditions of current operating parameter
The continuous type vacuum vapor deposition lithium equipment of card high speed carries out normal；
Four, cooling pressure release: after completing substrate vapor deposition lithium, closing crucible heater 10, unwinding system 3,4 and of substrate heater
Winding system 7 adjusts crucible lifting-transverse shifting platform 12, crucible 8 is moved on crucible fixed frame 9, using the cold mode of oil by earthenware
Crucible 8 is cooled to 40~50 DEG C, releases the vacuum pressure of upper cavity and lower chamber at this time；
Five, it takes substrate: opening the upper cavity and lower chamber of the continuous type vacuum vapor deposition lithium equipment of high speed, take out surface and steam
Plate lithium substrate.
Home roll 5 described in present embodiment is suspended in the top of crucible 8, is in a manner of the vapor deposition being deposited based on structure up and down.
Be deposited crucible above with home roll below distance be 5mm~20mm spacing, the diameter 450mm of home roll 5, length be 300mm~
1000mm；Crucible length is 100mm~800mm, and width is 20mm~150mm, and depth is 40mm~120mm, the crucible 8
The diameter ratio of width and home roll 5 is 1:(3~10), and be deposited crucible put it is consistent with home roll direction；This mode can be in base
Vapor deposition length is improved on material within the scope of 100m~3000m, for vapor deposition width to be adjustable within the scope of 100mm~1200mm, vapor deposition is thick
It can be adjusted at any time between 1 μm~100 μm of range of degree, 1 μm of tolerance+, lithium metal utilization rate can reach 90% or more, and homogeneity reaches
To ± 95% metallic lithium layer.
The relevant parameter of the continuous type vacuum vapor deposition lithium equipment of high speed described in present embodiment is as follows: substrate width is
100mm~1200mm；Vapor deposition width is 100mm~1200mm；Evaporation rate is 1m/min-50m/min, and LINEAR CONTINUOUS can
It adjusts；Vapor deposition length is 100m-3000m；Evaporation thickness is 1 μm~100 μm, 1 μm of tolerance+；Winding speed is 1m/min~80m/
Min, dynamic digital show speed；Equipment mobility > 98%, continuous coating thickness qualification rate > 99.5%；Lithium evaporation rate >=
200g/min。
Specific embodiment 9: one of present embodiment and specific embodiment one to eight difference are: institute in conjunction with Fig. 1
It states and temperature transmitter is set on the home roll 5 of the continuous type vacuum vapor deposition lithium equipment of high speed and home roll is silicon-controlled, become using temperature
Device and the silicon-controlled temperature by 5 surface substrate of home roll of home roll is sent to control at 80 DEG C or less.Other and specific embodiment one to eight
It is identical.
Specific embodiment 10: one of present embodiment and specific embodiment one to nine difference are: institute in conjunction with Fig. 1
The chill roll 6 for stating the continuous type vacuum vapor deposition lithium equipment of high speed connects silicon-controlled and cooler, utilizes silicon-controlled and cooler
It is 10 DEG C~20 DEG C by the control of 6 temperature of chill roll.Other are identical as specific embodiment one to nine.
Specific embodiment 11: in conjunction with Fig. 1, one of present embodiment and specific embodiment one to ten difference are:
Step 1 1. described in substrate wearing concrete operations it is as follows: first by substrate volume on the let off roll of unwinding system 3, then by substrate
It sequentially passes through and unreels transition roller 13, substrate heater 4, heating transition roller 14, home roll 5, cooling transition roller 15, chill roll 6 and receive
The wind-up roll of volume system 7, i.e. completion substrate wearing.Other are identical as specific embodiment one to ten.
The content of present invention is not limited only to the content of the respective embodiments described above, the group of one of them or several specific embodiments
The purpose of invention also may be implemented in contract sample.
Using following verification experimental verifications effect of the present invention
Embodiment 1: in conjunction with Fig. 1, the continuous type vacuum vapor deposition lithium equipment of high speed, it includes body fuselage 1, cavity dam
2, unwinding system 3, substrate heater 4, home roll 5, chill roll 6, winding system 7, crucible 8, crucible fixed frame 9, crucible heater
10, insulating layer 11, crucible lifting-transverse shifting platform 12, to unreel transition roller 13, heating transition roller 14, cooling transition roller 15, epicoele true
Empty valve 16, cavity of resorption vacuum valve 17 and charging visual windows 18；
The continuous type vacuum vapor deposition lithium equipment of high speed is separated into upper cavity under by cavity dam 2 and body fuselage 1
Cavity, the unwinding system 3, substrate heater 4, chill roll 6 and winding system 7 are arranged in the continuous type vacuum vapor deposition of high speed
In the upper cavity of lithium equipment, the transition roller 13 that unreels is arranged between unwinding system 3 and substrate heater 4, described heated
It crosses roller 14 to be arranged between home roll 5 and substrate heater 4, the cooling transition roller 15 is arranged between home roll 5 and chill roll 6；
The crucible 8, crucible fixed frame 9, crucible heater 10, insulating layer 11 and the setting of crucible lifting-transverse shifting platform 12 are continuous in high speed
In the lower chamber of type vacuum vapor deposition lithium equipment, the crucible fixed frame 9 is fixedly connected with 1 inner wall of body fuselage, the guarantor
Warm layer 11 is arranged on crucible lifting-transverse shifting platform 12, coats crucible heater 10 using insulating layer 11 and is used to keep the temperature, the earthenware
Crucible 8 is carried on crucible fixed frame 9, and when lithium is deposited, the crucible 8 is placed in crucible heater 10, and the top of the crucible 8
Portion is in curved surface parallel with home roll 5；Epicoele vacuum valve 16 is set on epicoele body sidewall, cavity of resorption is set in lower chamber side wall upper part
Charging visual windows 18 are arranged in lower chamber top side wall in vacuum valve 17；The home roll 5 is at cavity dam 2, a part
In upper cavity, another part is in lower chamber, and home roll 5 is 5mm~10mm at a distance from cavity dam 2；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes coating detection system, is examined using coating detection system
Survey chill roll 6 and cooling transition roller 15 and between substrate surface coating thickness；The coating detection system is the inspection of X-ray thickness
Survey instrument；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes pumped vacuum systems, using pumped vacuum systems to high speed
The upper cavity and lower chamber of continuous type vacuum vapor deposition lithium equipment carry out vacuumize process；The pumped vacuum systems includes machine
Tool vacuum pump, Roots vaccum pump and molecular pump；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes PLC control system, is controlled using PLC control system
The continuous type vacuum vapor deposition lithium equipment running of high speed；The PLC control system includes feeding and threading process, each parameter setting
Process, automatic running-substrate pre-add thermal flow process, automatic running-home roll heating procedure, automatic running-lithium material heating evaporation process,
It is cooling after automatic running-substrate conveying process, automatic running-continuous evaporating-plating thickness measuring and thickness control process, automatic running-vapor deposition
It is process, automatic running-tension force process, automatic running-tension force process, automatic running-winding uniformity process, automatic
Operation-winding uniformity process, automatic running-flattening process and automatic running-coiled strip surplus detection and shutdown process；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes crucible cooling system, the crucible cooling system packet
Containing cooling oil, crucible is silicon-controlled and crucible cooler, and the side wall of the crucible fixed frame 9 is hollow structure, and cooling oil is loaded in
In the hollow structure of 9 side wall of crucible fixed frame, it is cold that oil carried out to crucible 8 using cooling oil, using crucible is silicon-controlled and crucible is cold
But machine carries out circulating cooling to cooling oil；
The unwinding system includes let off roll, deviation-rectifying system, transition roller system, substrate evaporation rate control system, tension
Control system and flattening system；
The winding system includes wind-up roll, mechanical expansion shaft, AC driven motor, frequency-variable controller, SKF bearing, magnetic current
Body sealing and feeding turntable；
Temperature transmitter is set on the home roll 5 and home roll is silicon-controlled；
The chill roll 6 connects silicon-controlled and cooler；
The material of the body fuselage 1 is stainless steel, thickness 50mm；
The crucible 8 is semicircle or rectangle, and the diameter ratio of the width of the crucible 8 and home roll 5 is 1:3.75.
Embodiment 2: substrate vapor deposition lithium is realized using the continuous type vacuum vapor deposition lithium equipment of high speed described in embodiment 1
Method is specifically realized by the following steps:
One, the preparation stage: 1., first substrate is rolled up on the let off roll of unwinding system 3, then substrate is sequentially passed through and is unreeled
The winding of transition roller 13, substrate heater 4, heating transition roller 14, home roll 5, cooling transition roller 15, chill roll 6 and winding system 7
Roller, i.e. completion substrate are dressed, and closure upper cavity is under after substrate is worn in the continuous type vacuum vapor deposition lithium equipment of high speed
2., by lithium metal along charging visual windows 18 cavity is added in crucible 8, then crucible 8 is moved in crucible heater 10,
And crucible 8 put it is consistent with home roll direction, adjust crucible lifting-transverse shifting platform 12, make crucible 8 at a distance from 5 surface substrate of home roll
For 5mm, 3., to the continuous type vacuum vapor deposition lithium equipment of high speed it is sealed；
Two, it vacuumizes: the upper cavity of the continuous type vacuum vapor deposition lithium equipment of high speed being vacuumized, until the vacuum of upper cavity
Degree is 6.8 × 10-2Pa, while the lower chamber of the continuous type vacuum vapor deposition lithium equipment of high speed is vacuumized, until lower chambers is true
Reciprocal of duty cycle is 7 × 10-3Pa；
Three, it is deposited: starting crucible heater 10, and lithium metal temperature in real-time detection crucible 8, when lithium metal in crucible 8
When temperature reaches 350 DEG C, starting unwinding system 3, substrate heater 4 and winding system 7, the continuous take-up type vacuum of adjustment high speed steam
Lithium equipment operating parameter is plated, is protected until substrate surface lithium layer thickness reaches actual requirement, and under the conditions of current operating parameter
The continuous type vacuum vapor deposition lithium equipment of card high speed carries out normal；
Four, cooling pressure release: after completing substrate vapor deposition lithium, closing crucible heater 10, unwinding system 3,4 and of substrate heater
Winding system 7 adjusts crucible lifting-transverse shifting platform 12, crucible 8 is moved on crucible fixed frame 9, using the cold mode of oil by earthenware
Crucible 8 is cooled to 40~50 DEG C, releases the vacuum pressure of upper cavity and lower chamber at this time；
Five, it takes substrate: opening the upper cavity and lower chamber of the continuous type vacuum vapor deposition lithium equipment of high speed, take out surface and steam
Plate lithium substrate.
Home roll 5 described in the present embodiment is suspended in the top of crucible 8, is in a manner of the vapor deposition being deposited based on structure up and down.It steams
It plates above crucible and distance is 5mm spacing, the diameter 450mm of home roll 5, length 800mm below home roll；Crucible length is
800mm, width 120mm, depth 85mm.
The relevant parameter of the continuous type vacuum vapor deposition lithium equipment of high speed described in present embodiment is as follows: substrate width is
900mm；Vapor deposition width is 800mm；Evaporation rate is 16m/min (i.e. 5 revolving speed of home roll is 16m/min)；Vapor deposition length is 400m；
Evaporation thickness is 10 μm；Winding speed is 10m/min, and dynamic digital shows speed；Equipment mobility > 98%, continuous coating are thick
Spend qualification rate > 99.5%；Lithium evaporation rate >=200g/min.
Temperature transmitter and home roll are set on the home roll 5 of the continuous type vacuum vapor deposition lithium equipment of high speed described in the present embodiment
It is silicon-controlled, it is controlled using the silicon-controlled temperature by 5 surface substrate of home roll of temperature transmitter and home roll at 80 DEG C or less.
The chill roll 6 of the continuous type vacuum vapor deposition lithium equipment of high speed described in the present embodiment connects silicon-controlled and cooler,
Being controlled 6 temperature of chill roll using silicon-controlled and cooler is 10 DEG C~20 DEG C.
Other parameters are as follows:
1, facility environment temperature is room temperature；
2, facility environment humidity: dew point degree Celsius be -30 DEG C (when dew point degree Celsius is -30 DEG C indoor relative humidity be 1~
2%), because lithium metal can burn under room temperature humidity, equipment itself will be placed in dry environments；
3, the substrate wearing used time is 37min；
4, epicoele vacuum degree is 6.8 × 10-2Pa, epicoele vacuum values reach target value；
5, the epicoele pumpdown time is 13min；
6, cavity of resorption vacuum degree 7.0 × 10-3Pa, cavity of resorption vacuum values reach target value
7, the cavity of resorption pumpdown time is 33min；
8, substrate heating time is 5min；
9, substrate heating temperature is 80 DEG C；
10, crucible heating temperature is 400 °, and there is no problem for heating temperature, upper and lower temperature difference ± 5 DEG C；
11, crucible heating time is 22min；
12, crucible cooling time is 31min；
13, temperature is 46 DEG C after crucible is cooling；
14, home roll revolving speed is 16m/min, and home roll speed can make adjustment according to needs when plated film, range 6m/min~
80m/min；
15, home roll temperature is 70 DEG C~80 DEG C, and the source of home roll temperature is that evaporator crucible heating and vapor deposition process are received and absorbed
The heat arrived；
16, X-ray thickness gauge test 1 μm~100 μm of thickness range, film thickness gauge detection range value working range it
Interior, actual measured value is 10um thickness, deviation ± 5%；
17, epicoele venting duration is 8min；
18, cavity of resorption venting duration is 10min；
19, substrate cooling temperature is 31 DEG C, temperature-detecting device after setting vapor deposition, and detection substrate is cooling by chill roll 6
Actual temperature afterwards, Temperature estimate value should be within the scope of 100~150 DEG C after vapor deposition.By the cooling temperature of the cooling rear substrate of chill roll 6
Degree is 31 DEG C.
20, substrate cooling time is 5s；
21, evaporation time 28min；
22, evaporation thickness is 10 μm, and vapor deposition starts that head thickness is relatively low probably has 5m or so, is adjusted tape running speed
Afterwards, between 9.4 μm~10.5 μm of thickness range qualification；
23, coating uniformity is detected as within ± 10%；Time detects thickness deviation ± 5% or so；
24, vapor deposition length is 400m；
25, lithium metal utilization rate is 90.6%, 2kg lithium metal, and remaining 0.2kg, vapor deposition weight is 1.63kg, consumption
0.17kg。
Claims (10)
1. the continuous type vacuum vapor deposition lithium equipment of high speed, it is characterised in that continuously type vacuum vapor deposition lithium equipment includes high speed
Body fuselage (1), cavity dam (2), unwinding system (3), substrate heater (4), home roll (5), chill roll (6), winding system
(7), crucible (8), crucible fixed frame (9), crucible heater (10), insulating layer (11), crucible lifting-transverse shifting platform (12), unreel
Transition roller (13), heating transition roller (14), cooling transition roller (15), epicoele vacuum valve (16), cavity of resorption vacuum valve (17) and
It feeds visual windows (18)；
The continuous type vacuum vapor deposition lithium equipment of high speed is separated into upper cavity under by cavity dam (2) and body fuselage (1)
Cavity, the unwinding system (3), substrate heater (4), chill roll (6) and winding system (7) are arranged in the continuous takeup type of high speed
In the upper cavity of vacuum evaporation lithium equipment, it is described unreel transition roller (13) setting unwinding system (3) and substrate heater (4) it
Between, the heating transition roller (14) is arranged between home roll (5) and substrate heater (4), cooling transition roller (15) setting
Between home roll (5) and chill roll (6)；The crucible (8), crucible fixed frame (9), crucible heater (10), insulating layer (11)
It is arranged in the lower chamber of the continuous type vacuum vapor deposition lithium equipment of high speed with crucible lifting-transverse shifting platform (12), the crucible is solid
To determine frame (9) to be fixedly connected with body fuselage (1) inner wall, the insulating layer (11) is arranged on crucible lifting-transverse shifting platform (12),
Using insulating layer (11) cladding crucible heater (10) for keeping the temperature, the crucible (8) is carried on crucible fixed frame (9), when
When lithium is deposited, the crucible (8) is placed in crucible heater (10), and the top of the crucible (8) and home roll (5) are in curved surface flat
Row, crucible (8) put it is consistent with home roll direction, adjust crucible lifting-transverse shifting platform (12), make crucible (8) and home roll (5) surface
The distance of substrate is 5mm~20mm；Epicoele vacuum valve (16) are set on epicoele body sidewall, are arranged in lower chamber side wall upper part
Charging visual windows (18) is arranged in lower chamber top side wall in cavity of resorption vacuum valve (17)；The home roll (5) passes through cavity dam
(2), in upper cavity, another part is in lower chamber a part, and home roll (5) is 5mm at a distance from cavity dam (2)
~10mm；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes coating detection system, is detected using coating detection system cold
But substrate surface coating thickness between roller (6) and cooling transition roller (15)；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes pumped vacuum systems, continuous to high speed using pumped vacuum systems
The upper cavity and lower chamber of type vacuum vapor deposition lithium equipment carry out vacuumize process；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes PLC control system, controls high speed using PLC control system
Continuous type vacuum vapor deposition lithium equipment running；
The continuous type vacuum vapor deposition lithium equipment of high speed further includes crucible cooling system, and the crucible cooling system includes cold
But oil, crucible is silicon-controlled and crucible cooler, the side wall of the crucible fixed frame (9) is hollow structure, and cooling oil is loaded in earthenware
In the hollow structure of crucible fixed frame (9) side wall, it is cold that oil carried out to crucible (8) using cooling oil, using crucible is silicon-controlled and crucible
Cooler carries out circulating cooling to cooling oil.
2. the continuous type vacuum vapor deposition lithium equipment of high speed according to claim 1, it is characterised in that the unwinding system
(3) comprising let off roll, deviation-rectifying system, transition roller system, substrate evaporation rate control system, tension control system and flattening system
System.
3. the continuous type vacuum vapor deposition lithium equipment of high speed according to claim 1, it is characterised in that the winding system
It (7) include wind-up roll, mechanical expansion shaft, AC driven motor, frequency-variable controller, SKF bearing, magnet fluid sealing and feeding turntable.
4. the continuous type vacuum vapor deposition lithium equipment of high speed according to claim 1, it is characterised in that on the home roll (5)
Temperature transmitter is set and home roll is silicon-controlled.
5. the continuous type vacuum vapor deposition lithium equipment of high speed according to claim 1, it is characterised in that the chill roll (6)
Connect silicon-controlled and cooler.
6. the continuous type vacuum vapor deposition lithium equipment of high speed according to claim 1, it is characterised in that the body fuselage
(1) material is stainless steel, thickness 50mm.
7. the continuous type vacuum vapor deposition lithium equipment of high speed according to claim 1, it is characterised in that the crucible (8) is
Semicircle or rectangle；And the width of the crucible (8) and the diameter ratio of home roll (5) are 1:(3~10).
8. the method for realizing substrate vapor deposition lithium using the continuous type vacuum vapor deposition lithium equipment of high speed described in claim 1,
Being characterized by the method that the continuous type vacuum vapor deposition lithium equipment of high speed realizes substrate vapor deposition lithium is to complete according to the following steps
:
One, the preparation stage: after 1., by substrate being worn in the continuous type vacuum vapor deposition lithium equipment of high speed closure upper cavity and under
2., by lithium metal along charging visual windows (18) cavity is added in crucible (8), crucible (8) is then moved to crucible heater
(10) on, and crucible (8) put it is consistent with home roll direction, adjust crucible lifting-transverse shifting platform (12), make crucible (8) and home roll
(5) distance of surface substrate is 5mm~20mm, 3., to the continuous type vacuum vapor deposition lithium equipment of high speed is sealed；
Two, it vacuumizes: the upper cavity of the continuous type vacuum vapor deposition lithium equipment of high speed being vacuumized, until the vacuum degree of upper cavity is
6.5×10-2Pa~7 × 10-2Until Pa, while the lower chamber of the continuous type vacuum vapor deposition lithium equipment of high speed is vacuumized, until
The vacuum degree of lower chambers is 7 × 10-3Pa~7 × 10-4Until Pa；
Three, it is deposited: starting crucible heater (10), and the interior lithium metal temperature of real-time detection crucible (8), when crucible (8) interior metal
When lithium temperature reaches 350 DEG C, starting unwinding system (3), substrate heater (4) and winding system (7), the continuous winding of adjustment high speed
Formula vacuum evaporation lithium equipment operating parameter, until substrate surface lithium layer thickness reaches actual requirement, and in current operating parameter
Under the conditions of to guarantee that the continuous type vacuum vapor deposition lithium equipment of high speed carries out normal；
Four, cooling pressure release: after completing substrate vapor deposition lithium, closing crucible heater (10), unwinding system (3), substrate heater (4)
With winding system (7), adjusts crucible lifting-transverse shifting platform (12), crucible (8) is moved on crucible fixed frame (9), using oil
Crucible (8) are cooled to 40~50 DEG C by cold mode, release the vacuum pressure of upper cavity and lower chamber at this time；
Five, it takes substrate: opening the upper cavity and lower chamber of the continuous type vacuum vapor deposition lithium equipment of high speed, take out surface and lithium is deposited
Substrate.
9. the side according to claim 8 for realizing substrate vapor deposition lithium using the continuous type vacuum vapor deposition lithium equipment of high speed
Method, it is characterised in that temperature transmitter and home roll are set on the home roll (5) of the continuous type vacuum vapor deposition lithium equipment of high speed
It is silicon-controlled, it is controlled using the silicon-controlled temperature by home roll (5) surface substrate of temperature transmitter and home roll at 80 DEG C or less；The height
The chill roll (6) of fast continuous type vacuum vapor deposition lithium equipment connects silicon-controlled and cooler, will using silicon-controlled and cooler
The control of chill roll (6) temperature is 10 DEG C~20 DEG C.
10. the side according to claim 8 for realizing substrate vapor deposition lithium using the continuous type vacuum vapor deposition lithium equipment of high speed
Method, it is characterised in that step 1 1. described in substrate wearing concrete operations it is as follows: first by substrate roll up unreeling in unwinding system (3)
On roller, then substrate is sequentially passed through and unreels transition roller (13), substrate heater (4), heating transition roller (14), home roll (5), cold
But the wind-up roll of transition roller (15), chill roll (6) and winding system (7), i.e. completion substrate wearing.
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| CN201710438908.4A CN107177820B (en) | 2017-06-12 | 2017-06-12 | Method high speed continuous type vacuum vapor deposition lithium equipment and realize substrate vapor deposition lithium using it |
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|---|---|---|---|
| CN201710438908.4A CN107177820B (en) | 2017-06-12 | 2017-06-12 | Method high speed continuous type vacuum vapor deposition lithium equipment and realize substrate vapor deposition lithium using it |
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| CN107177820B true CN107177820B (en) | 2019-05-24 |
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| CN111058000B (en) * | 2019-12-25 | 2022-06-24 | 复阳固态储能科技(溧阳)有限公司 | High-speed volume to volume vacuum lithium film apparatus for producing of tertiary evaporation |
| CN111378952A (en) * | 2020-04-29 | 2020-07-07 | 义乌市森煌科技有限公司 | Winding type film coating machine |
| CN112877670A (en) * | 2021-02-06 | 2021-06-01 | 合肥市辉耀真空材料有限责任公司 | Bead-planted film vacuum evaporation equipment with crucible as evaporation source and film coating process |
| CN114824179A (en) * | 2022-04-28 | 2022-07-29 | 南昌大学 | Preparation method of solid-state lithium battery |
| WO2024011536A1 (en) * | 2022-07-14 | 2024-01-18 | 扬州纳力新材料科技有限公司 | Copper composite current collector, preparation method therefor and application thereof |
| CN115563665B (en) * | 2022-09-29 | 2023-07-21 | 北京中科科美科技股份有限公司 | Dynamic calculation method of P/T change process based on vacuum system |
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