CN107177820A - High-speed and continuous type vacuum vapor deposition lithium equipment and the method that base material evaporation lithium is realized using it - Google Patents
High-speed and continuous type vacuum vapor deposition lithium equipment and the method that base material evaporation lithium is realized using it Download PDFInfo
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- CN107177820A CN107177820A CN201710438908.4A CN201710438908A CN107177820A CN 107177820 A CN107177820 A CN 107177820A CN 201710438908 A CN201710438908 A CN 201710438908A CN 107177820 A CN107177820 A CN 107177820A
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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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- Battery Electrode And Active Subsutance (AREA)
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Abstract
High-speed and continuous type vacuum vapor deposition lithium equipment and the method that base material evaporation lithium is realized using it, it is related to a kind of base material evaporation lithium equipment and realizes the method that lithium is deposited in base material using it.Low to the utilization rate of lithium metal the invention aims to solve existing base material evaporation lithium equipment, evaporation thickness is≤1 μm, the problem of pollution range is big during evaporation.High-speed and continuous type vacuum vapor deposition lithium equipment include body fuselage, cavity dam, unreel system, substrate heater, home roll, chill roll, winding system, crucible, crucible fixed mount, crucible heater, heat-insulation 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；Method：Ensure to adjust at any time between 1 μm~100 μm of evaporation thickness scope, lithium metal optimum rate of utilization can reach more than 90%.Lithium is deposited present invention is mainly used for base material.
Description
Technical field
The method that lithium is deposited in base material is realized the present invention relates to a kind of base material evaporation lithium equipment and using it.
Background technology
Elemental lithium material property is：Lithium be easy to the chemical combination such as oxygen, nitrogen, sulphur, meet water burning, storage condition strictly waits special
Point, so can only carry out being heated into gaseous state evaporation to lithium metal in the case of high vacuum.Existing large scale equipment be AM aluminum metallization, nickel,
The materials such as zinc, and small-sized evaporation metal lithium equipment utilization rate there was only 2%~10% between, evaporation thickness be≤1 μm, if
Evaporation thickness increase, is deposited in chamber when uniformity can not ensure and be deposited and is full of lithium steam, the big grade of pollution range lacks during evaporation
Point.
The content of the invention
It is low to the utilization rate of lithium metal the invention aims to solve existing base material evaporation lithium equipment, evaporation thickness for≤
1 μm, the problem of pollution range is big during evaporation, and high-speed and continuous type vacuum vapor deposition lithium equipment is provided and base material is realized using it
The method of lithium is deposited.
High-speed and continuous type vacuum vapor deposition lithium equipment, it includes body fuselage, cavity dam, unreels system, base material and add
Hot device, home roll, chill roll, winding system, crucible, crucible fixed mount, crucible heater, heat-insulation 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；
High-speed and continuous type vacuum vapor deposition lithium equipment is separated into upper cavity and cavity of resorption by cavity dam and body fuselage
Body, system, substrate heater, chill roll and the winding system of unreeling is arranged on high-speed and continuous type vacuum vapor deposition lithium equipment
Upper cavity in, the transition roller that unreels is arranged between the system of unreeling and substrate heater, it is described heating transition roller be arranged on
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, heat-insulation layer and crucible lifting-transverse shifting platform are arranged under high-speed and continuous type vacuum vapor deposition lithium equipment
In cavity, the crucible fixed mount is fixedly connected with body fuselage inwall, and the heat-insulation layer is arranged on crucible lifting-transverse shifting platform
On, the crucible is carried on crucible fixed mount, 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；It is used to be incubated using heat-insulation layer cladding crucible heater；On being set on epicoele body sidewall
Chamber vacuum valve, cavity of resorption vacuum valve is set in lower chamber side wall upper part, and charging visual windows are set 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 high-speed and continuous type vacuum vapor deposition lithium equipment also includes coating detecting system, is examined using coating detecting system
Survey chill roll and cooling transition roller and between substrate surface coating thickness；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes pumped vacuum systems, using pumped vacuum systems at a high speed
The upper cavity and lower chamber of continuous type vacuum vapor deposition lithium equipment carry out vacuumize process；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes PLC control system, is controlled using PLC control system
High-speed and continuous type vacuum vapor deposition lithium equipment is operated；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes crucible cooling system, the crucible cooling system bag
Containing cooling oil, crucible controllable silicon and crucible cooler, the side wall of the crucible fixed mount is hollow structure, and cooling oil is loaded in earthenware
In the hollow structure of crucible fixed mount side wall, oil cooling is carried out to crucible using cooling oil, crucible controllable silicon and crucible cooler is utilized
Circulating cooling is carried out to cooling oil.
The method that lithium is deposited in base material is realized using high-speed and continuous type vacuum vapor deposition lithium equipment, is specifically according to the following steps
Complete：
First, the preparatory stage：1. closure upper cavity after, base material is worn in high-speed and continuous type vacuum vapor deposition lithium equipment
And lower chamber, 2., by lithium metal add in crucible, crucible is moved in crucible heater along charging visual windows then, and
Crucible is put consistent with home roll direction, adjusts crucible lifting-transverse shifting platform, make the distance of crucible and home roll surface substrate for 5mm~
20mm, 3., to high-speed and continuous type vacuum vapor deposition lithium equipment is sealed；
2nd, vacuumize：The upper cavity of high-speed and continuous type vacuum vapor deposition lithium equipment is vacuumized, to the vacuum of upper cavity
Spend for 6.5 × 10-2Pa~7 × 10-2Untill Pa, while being taken out very to the lower chamber of high-speed and continuous type vacuum vapor deposition lithium equipment
Sky, the vacuum to lower chambers is 7 × 10-3Pa~7 × 10-4Untill Pa；
3rd, it is deposited：Start crucible heater, and lithium metal temperature in detection crucible in real time, when lithium metal temperature in crucible
When reaching 350 DEG C, startup unreels system, substrate heater and winding system, and adjustment high-speed and continuous type vacuum vapor deposition lithium is set
Standby operational factor, ensures at a high speed untill substrate surface lithium layer thickness reaches actual requirement, and under the conditions of current operating parameter
Continuous type vacuum vapor deposition lithium equipment carries out normal；
4th, pressure release is cooled down：Complete after base material evaporation lithium, closing crucible heater, unreel system, substrate heater and winding
System, adjusts crucible lifting-transverse shifting platform, crucible is moved on crucible fixed mount, crucible is cooled into 40 using oil cooling mode
~50 DEG C, now release the vacuum pressure of upper cavity and lower chamber；
5th, base material is taken：The upper cavity and lower chamber of high-speed and continuous type vacuum vapor deposition lithium equipment are opened, surface is taken out and steams
Plate lithium base material.
Advantage of the present invention：First, set high-speed and continuous type vacuum vapor deposition lithium equipment by cavity dam and body fuselage
Upper cavity and lower chamber are separated into, prevents that lithium steam pollutes to base material during evaporation, and the vacuum of upper cavity is 6.5 during evaporation lithium
×10-2Pa~7 × 10-2Pa, the vacuum of lower chambers is 7 × 10-3Pa~7 × 10-4Pa；The high vacuum values of lower evaporation chamber can be carried
The adhesive force of high lithium and base material, and suppress lithium to epicoele pollution there is provided advantage；2nd, evaporation crucible and base material distance are
5mm~20mm spacing, and be deposited crucible put it is consistent with home roll direction, it is ensured that can between 1 μm~100 μm of evaporation thickness scope
Adjust at any time, 1 μm of tolerance+, the effective utilization rate for improving lithium metal, lithium metal optimum rate of utilization can reach more than 90%, section
Cost-saving, and homogeneity reaches ± 95%；3rd, high-speed and continuous type vacuum vapor deposition lithium equipment of the present invention has explosion-proof, sealing
Property good, anti-high pressure, high-temperature heating, cooling down and automatic detection steam thickness of coating function, are large-scale continuous safety in production
The favourable guarantee provided.
Brief description of the drawings
Fig. 1 is high-speed and continuous type vacuum vapor deposition lithium device structure schematic diagram described in embodiment one.
Embodiment
Embodiment one：With reference to Fig. 1, present embodiment is high-speed and continuous type vacuum vapor deposition lithium equipment, and it is wrapped
Include body fuselage 1, cavity dam 2, unreel system 3, substrate heater 4, home roll 5, chill roll 6, winding system 7, crucible 8, earthenware
Crucible fixed mount 9, crucible heater 10, heat-insulation layer 11, crucible lifting-transverse shifting platform 12, unreel transition roller 13, heating transition roller 14,
Cool down transition roller 15, epicoele vacuum valve 16, cavity of resorption vacuum valve 17 and charging visual windows 18；
High-speed and continuous type vacuum vapor deposition lithium equipment is separated into upper cavity with by cavity dam 2 and body fuselage 1
Cavity, system 3, substrate heater 4, chill roll 6 and the winding system 7 of unreeling is arranged on high-speed and continuous type vacuum vapor deposition
In the upper cavity of lithium equipment, the transition roller 13 that unreels is arranged between the system of unreeling 3 and substrate heater 4, described heated
Cross 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 mount 9, crucible heater 10, heat-insulation layer 11 and crucible lifting-transverse shifting platform 12 are arranged on high-speed and continuous
In the lower chamber of type vacuum vapor deposition lithium equipment, the crucible fixed mount 9 is fixedly connected with the inwall of body fuselage 1, described to protect
Warm layer 11 is arranged on crucible lifting-transverse shifting platform 12, is used to be incubated using the cladding crucible heater 10 of heat-insulation layer 11, the earthenware
Crucible 8 is carried on crucible fixed mount 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
Vacuum valve 17, charging visual windows 18 are set in lower chamber top side wall；The home roll 5 is passed through at cavity dam 2, a part
In upper cavity, another part is in lower chamber, and the distance of home roll 5 and cavity dam 2 is 5mm~10mm；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes coating detecting system, is examined using coating detecting system
Survey chill roll 6 and cooling transition roller 15 and between substrate surface coating thickness；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes pumped vacuum systems, using pumped vacuum systems at a high speed
The upper cavity and lower chamber of continuous type vacuum vapor deposition lithium equipment carry out vacuumize process；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes PLC control system, is controlled using PLC control system
High-speed and continuous type vacuum vapor deposition lithium equipment is operated；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes crucible cooling system, the crucible cooling system bag
Containing cooling oil, crucible controllable silicon and crucible cooler, the side wall of the crucible fixed mount 9 is hollow structure, and cooling oil is loaded in
In the hollow structure of the side wall of crucible fixed mount 9, oil cooling is carried out to crucible 8 using cooling oil, it is cold using crucible controllable silicon and crucible
But machine carries out circulating cooling to cooling oil.
Fig. 1 is 1 expression in high-speed and continuous type vacuum vapor deposition lithium device structure schematic diagram, figure described in present embodiment one
Body fuselage, 2 represent cavity dam, and 3 represent to unreel system, and 4 represent base material heating, and 5 represent home roll, and 6 represent chill roll, 7 tables
Show winding system, 8 represent crucible, and 9 represent crucible fixed mount, and 10 represent crucible heater, and 11 represent heat-insulation layer, and 12 represent crucible
Lifting-transverse shifting platform, 13 represent to unreel transition roller, and 14 represent heating transition roller, and 15 represent cooling transition roller, and 16 represent that epicoele is true
Empty valve, 17 represent cavity of resorption vacuum valve, and 18 represent charging visual windows.
Coating detecting system described in present embodiment is X-ray thickness gauges.
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 comprising feeding and threading flow, each parameter setting flow, automatic running-
Base material pre-add thermal flow process, automatic running-home roll heating procedure, automatic running-lithium material heating evaporation flow, automatic running-base material
Cooling process, automatic fortune after conveying flow, automatic running-continuous evaporating-plating thickness measuring and thickness control flow, automatic running-evaporation
Row-tension force flow, automatic running-tension force flow, automatic running-winding regularity flow, automatic running-winding are whole
Neat degree flow, automatic running-flattening flow and automatic running-coiled strip surplus detection are with shutting down flow.
Principle of the high-speed and continuous type vacuum vapor deposition lithium equipment as other vacuum coating equipments, is required in high vacuum
Good evaporation effect is obtained under state, high-speed and continuous type vacuum vapor deposition lithium equipment is company due to its special operation principle
Continuous evaporation, often vacuum chamber is more much bigger than common coating machine spatial volume, it is necessary to be coiling chamber with the opposing spaced apart of cavity dam 2
(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, because the distance of home roll 5 and cavity dam 2 is 5mm~10mm, base material thickness is micron order, therefore base material passes through master
Crack turnover coiling chamber and vaporization chamber between roller 5 and cavity dam 2.Coiling chamber is continuously working due to there is the presence of basement membrane
During, basement membrane is in itself and interlayer discharge quantity is very big, and the discharge quantity of vaporization chamber is relatively small.Coiling chamber and vaporization chamber are two phases
To independent space, and both vavuum pumps of configuration are variant；What coiling chamber master took out pump configuration is the less vacuum of relative pumping speed
Pump, what vaporization chamber master took out pump configuration is relative pumping speed very big vavuum pump, although be connection between two chamber bodies, but due to master
The distance of roller 5 and cavity dam 2 is 5mm~10mm, and the vacuum difference existed between crack effect, two rooms is obvious
's；Because evaporation material is that gas procedure is present, it is necessary to worked under higher vacuum degree condition in vaporization chamber, 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.In addition wind
Vavuum pump is separately separately configured in room and vaporization chamber, also there is cost-effective consideration.If necessary to which coiling chamber is also maintained at into Gao Zhen
Reciprocal of duty cycle, the pump of configuration is accomplished by bigger pumping speed, and cost performance is not high.
Embodiment two：With reference to Fig. 1, the difference of present embodiment and embodiment one is：It is described to unreel
System includes let off roll, deviation-rectifying system, transition roller system, base material evaporation rate control system, tension control system and flattening system
System.Other are identical with embodiment one.
Embodiment three：With reference to Fig. 1, one of present embodiment and embodiment one or two difference are：Institute
State winding system comprising wind-up roll, mechanical expansion shaft, AC driven motor, frequency-variable controller, SKF bearings, magnet fluid sealing and on
Expect turntable.Other are identical with embodiment one or two.
Embodiment four：With reference to Fig. 1, one of present embodiment and embodiment one to three difference are：Institute
State and temperature transmitter and home roll controllable silicon are set on home roll 5.Other are identical with embodiment one to three.
Embodiment five：With reference to Fig. 1, one of present embodiment and embodiment one to four difference are：Institute
State the connection controllable silicon of chill roll 6 and cooler.Other are identical with embodiment one to four.
Embodiment six：With reference to Fig. 1, one of present embodiment and embodiment one to five difference are：Institute
The material for stating body fuselage 1 is stainless steel, thickness 50mm.Other are identical with embodiment one to five.
Embodiment seven：With reference to Fig. 1, one of present embodiment and embodiment one to six difference are：Institute
It is semicircle or rectangle to state crucible 8, and the width of the crucible 8 and the diameter ratio of home roll 5 are 1:(3~10).Other and tool
Body embodiment one to six is identical.
Embodiment eight：With reference to Fig. 1, present embodiment utilizes the high-speed and continuous described in embodiment one to seven
Type vacuum vapor deposition lithium equipment realizes the method that lithium is deposited in base material, is specifically realized by the following steps：
First, the preparatory stage：1. closure upper cavity after, base material is worn in high-speed and continuous type vacuum vapor deposition lithium equipment
And lower chamber, 2., by lithium metal added along charging visual windows 18 in crucible 8, crucible 8 is then moved to crucible heater 10
On, and crucible 8 puts, adjustment crucible lifting-transverse shifting platform 12 consistent with home roll direction, makes crucible 8 and the surface substrate of home roll 5
Distance is 5mm~20mm, 3., to high-speed and continuous type vacuum vapor deposition lithium equipment is sealed；
2nd, vacuumize：The upper cavity of high-speed and continuous type vacuum vapor deposition lithium equipment is vacuumized, to the vacuum of upper cavity
Spend for 6.5 × 10-2Pa~7 × 10-2Untill Pa, while being taken out very to the lower chamber of high-speed and continuous type vacuum vapor deposition lithium equipment
Sky, the vacuum to lower chambers is 7 × 10-3Pa~7 × 10-4Untill Pa；
3rd, it is deposited：Start crucible heater 10, and lithium metal temperature in detection crucible 8 in real time, when lithium metal in crucible 8
When temperature reaches 350 DEG C, startup unreels system 3, substrate heater 4 and winding system 7, and adjustment high-speed and continuous take-up type vacuum steams
Lithium equipment operational factor is plated, is protected untill substrate surface lithium layer thickness reaches actual requirement, and under the conditions of current operating parameter
High-speed and continuous type vacuum vapor deposition lithium equipment is demonstrate,proved to carry out normally；
4th, pressure release is cooled down：Complete after base material evaporation lithium, closing crucible heater 10, unreel system 3, the and of substrate heater 4
Winding system 7, adjustment crucible lifting-transverse shifting platform 12, crucible 8 is moved on crucible fixed mount 9, using oil cooling mode by earthenware
Crucible 8 is cooled to 40~50 DEG C, now releases the vacuum pressure of upper cavity and lower chamber；
5th, base material is taken：The upper cavity and lower chamber of high-speed and continuous type vacuum vapor deposition lithium equipment are opened, surface is taken out and steams
Plate lithium base material.
Home roll 5 described in present embodiment is suspended in the top of crucible 8, is the evaporation mode based on evaporation 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
Evaporation length is improved on material in the range of 100m~3000m, evaporation width is adjustable in the range of 100mm~1200mm, and evaporation is thick
It can be adjusted at any time between 1 μm~100 μm of scope of degree, 1 μm of tolerance+, lithium metal utilization rate can reach more than 90%, and homogeneity reaches
To ± 95% metallic lithium layer.
The relevant parameter of high-speed and continuous type vacuum vapor deposition lithium equipment is as follows described in present embodiment：Substrate width is
100mm~1200mm；Evaporation width is 100mm~1200mm；Evaporation rate is 1m/min-50m/min, and LINEAR CONTINUOUS can
Adjust；Evaporation length is 100m-3000m；Evaporation thickness is 1 μm~100 μm, 1 μm of tolerance+；Winding speed is 1m/min~80m/
Min, dynamic digital display speed；Equipment mobility ＞ 98%, continuous coating thickness qualification rate ＞ 99.5%；Lithium evaporation rate >=
200g/min。
Embodiment nine：With reference to Fig. 1, one of present embodiment and embodiment one to eight difference are：Institute
State and temperature transmitter and home roll controllable silicon are set on the home roll 5 of high-speed and continuous type vacuum vapor deposition lithium equipment, become using temperature
Send device and home roll controllable silicon by the temperature control of the surface substrate of home roll 5 below 80 DEG C.Other and embodiment one to eight
It is identical.
Embodiment ten：With reference to Fig. 1, one of present embodiment and embodiment one to nine difference are：Institute
The connection controllable silicon of chill roll 6 and cooler of high-speed and continuous type vacuum vapor deposition lithium equipment are stated, controllable silicon and cooler is utilized
It it is 10 DEG C~20 DEG C by the temperature control of chill roll 6.Other are identical with embodiment one to nine.
Embodiment 11：With reference to Fig. 1, one of present embodiment and embodiment one to ten difference are：
Step one 1. described in base material wearing concrete operations it is as follows：First by base material volume on the let off roll of the system that unreels 3, then by base material
Sequentially pass through and unreel 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, that is, complete base material wearing.Other are identical with embodiment one to ten.
Present invention is not limited only to the content of the respective embodiments described above, the group of one of them or several embodiments
Contract sample can also realize the purpose of invention.
Using following verification experimental verifications effect of the present invention
Embodiment 1：With reference to Fig. 1, high-speed and continuous type vacuum vapor deposition lithium equipment, it includes body fuselage 1, cavity dam
2nd, system 3, substrate heater 4, home roll 5, chill roll 6, winding system 7, crucible 8, crucible fixed mount 9, crucible heater are unreeled
10th, heat-insulation 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；
High-speed and continuous type vacuum vapor deposition lithium equipment is separated into upper cavity with by cavity dam 2 and body fuselage 1
Cavity, system 3, substrate heater 4, chill roll 6 and the winding system 7 of unreeling is arranged on high-speed and continuous type vacuum vapor deposition
In the upper cavity of lithium equipment, the transition roller 13 that unreels is arranged between the system of unreeling 3 and substrate heater 4, described heated
Cross 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 mount 9, crucible heater 10, heat-insulation layer 11 and crucible lifting-transverse shifting platform 12 are arranged on high-speed and continuous
In the lower chamber of type vacuum vapor deposition lithium equipment, the crucible fixed mount 9 is fixedly connected with the inwall of body fuselage 1, described to protect
Warm layer 11 is arranged on crucible lifting-transverse shifting platform 12, is used to be incubated using the cladding crucible heater 10 of heat-insulation layer 11, the earthenware
Crucible 8 is carried on crucible fixed mount 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
Vacuum valve 17, charging visual windows 18 are set in lower chamber top side wall；The home roll 5 is passed through at cavity dam 2, a part
In upper cavity, another part is in lower chamber, and the distance of home roll 5 and cavity dam 2 is 5mm~10mm；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes coating detecting system, is examined using coating detecting system
Survey chill roll 6 and cooling transition roller 15 and between substrate surface coating thickness；Described coating detecting system is examined for X-ray thickness
Survey instrument；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes pumped vacuum systems, using pumped vacuum systems at a high speed
The upper cavity and lower chamber of continuous type vacuum vapor deposition lithium equipment carry out vacuumize process；Described pumped vacuum systems includes machine
Tool vavuum pump, Roots vaccum pump and molecular pump；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes PLC control system, is controlled using PLC control system
High-speed and continuous type vacuum vapor deposition lithium equipment is operated；The PLC control system includes feeding and threading flow, each parameter setting
Flow, automatic running-base material pre-add thermal flow process, automatic running-home roll heating procedure, automatic running-lithium material heating evaporation flow,
Cooled down after automatic running-base material conveying flow, automatic running-continuous evaporating-plating thickness measuring and thickness control flow, automatic running-evaporation
It is flow, automatic running-tension force flow, automatic running-tension force flow, automatic running-winding regularity flow, automatic
Operation-winding regularity flow, automatic running-flattening flow and automatic running-coiled strip surplus detection are with shutting down flow；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes crucible cooling system, the crucible cooling system bag
Containing cooling oil, crucible controllable silicon and crucible cooler, the side wall of the crucible fixed mount 9 is hollow structure, and cooling oil is loaded in
In the hollow structure of the side wall of crucible fixed mount 9, oil cooling is carried out to crucible 8 using cooling oil, it is cold using crucible controllable silicon and crucible
But machine carries out circulating cooling to cooling oil；
The system that unreels includes let off roll, deviation-rectifying system, transition roller system, base material evaporation rate control system, tension force
Control system and flattening system；
The winding system includes wind-up roll, mechanical expansion shaft, AC driven motor, frequency-variable controller, SKF bearings, magnetic current
Body is sealed and feeding turntable；
Temperature transmitter and home roll controllable silicon are set on the home roll 5；
The connection controllable silicon of chill roll 6 and cooler；
The material of the body fuselage 1 is stainless steel, thickness 50mm；
The crucible 8 is semicircle or rectangle, and the width of the crucible 8 and the diameter ratio of home roll 5 are 1:3.75.
Embodiment 2：Base material evaporation lithium is realized using the high-speed and continuous type vacuum vapor deposition lithium equipment described in embodiment 1
Method, is specifically realized by the following steps：
First, the preparatory stage：1., first by base material volume on the let off roll of the system that unreels 3, then base material is sequentially passed through and unreeled
Transition roller 13, substrate heater 4, heating transition roller 14, home roll 5, the winding for cooling down transition roller 15, chill roll 6 and winding system 7
Roller, that is, complete base material wearing, and closure upper cavity is with after base material is worn in high-speed and continuous type vacuum vapor deposition lithium equipment
Cavity, 2., by lithium metal adds in crucible 8 along charging visual windows 18, then crucible 8 is moved in crucible heater 10,
And crucible 8 puts, adjustment crucible lifting-transverse shifting platform 12 consistent with home roll direction, makes the distance of crucible 8 and the surface substrate of home roll 5
For 5mm, 3., to high-speed and continuous type vacuum vapor deposition lithium equipment seal；
2nd, vacuumize：The upper cavity of high-speed and continuous type vacuum vapor deposition lithium equipment is vacuumized, to the vacuum of upper cavity
Spend for 6.8 × 10-2Pa is true to lower chambers while vacuumized to the lower chamber of high-speed and continuous type vacuum vapor deposition lithium equipment
Reciprocal of duty cycle is 7 × 10-3Pa；
3rd, it is deposited：Start crucible heater 10, and lithium metal temperature in detection crucible 8 in real time, when lithium metal in crucible 8
When temperature reaches 350 DEG C, startup unreels system 3, substrate heater 4 and winding system 7, and adjustment high-speed and continuous take-up type vacuum steams
Lithium equipment operational factor is plated, is protected untill substrate surface lithium layer thickness reaches actual requirement, and under the conditions of current operating parameter
High-speed and continuous type vacuum vapor deposition lithium equipment is demonstrate,proved to carry out normally；
4th, pressure release is cooled down：Complete after base material evaporation lithium, closing crucible heater 10, unreel system 3, the and of substrate heater 4
Winding system 7, adjustment crucible lifting-transverse shifting platform 12, crucible 8 is moved on crucible fixed mount 9, using oil cooling mode by earthenware
Crucible 8 is cooled to 40~50 DEG C, now releases the vacuum pressure of upper cavity and lower chamber；
5th, base material is taken：The upper cavity and lower chamber of high-speed and continuous type vacuum vapor deposition lithium equipment are opened, surface is taken out and steams
Plate lithium base material.
Home roll 5 described in the present embodiment is suspended in the top of crucible 8, is the evaporation mode based on evaporation structure up and down.Steam
Plate crucible above with home roll below distance be 5mm spacing, the diameter 450mm of home roll 5, length is 800mm；Crucible length is
800mm, width is 120mm, and depth is 85mm.
The relevant parameter of high-speed and continuous type vacuum vapor deposition lithium equipment is as follows described in present embodiment：Substrate width is
900mm；Evaporation width is 800mm；Evaporation rate is 16m/min (i.e. the rotating speed of home roll 5 is 16m/min)；Evaporation length is 400m；
Evaporation thickness is 10 μm；Winding speed is 10m/min, dynamic digital display speed；Equipment mobility ＞ 98%, continuous coating is thick
Spend qualification rate ＞ 99.5%；Lithium evaporation rate >=200g/min.
Temperature transmitter and home roll are set described in the present embodiment on the home roll 5 of high-speed and continuous type vacuum vapor deposition lithium equipment
Controllable silicon, using temperature transmitter and home roll controllable silicon by the temperature control of the surface substrate of home roll 5 below 80 DEG C.
The connection controllable silicon of chill roll 6 and cooler of high-speed and continuous type vacuum vapor deposition lithium equipment described in the present embodiment,
By the temperature control of chill roll 6 it is 10 DEG C~20 DEG C using controllable silicon and cooler.
Other specification is as follows：
1st, facility environment temperature is room temperature；
2nd, 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 normal temperature humidity, equipment will be placed in dry environments in itself；
3rd, the base material wearing used time is 37min；
4th, epicoele vacuum is 6.8 × 10-2Pa, epicoele vacuum values reach desired value；
5th, the epicoele pumpdown time is 13min；
6th, cavity of resorption vacuum 7.0 × 10-3Pa, cavity of resorption vacuum values reach desired value
7th, the cavity of resorption pumpdown time is 33min；
8th, the base material heat time is 5min；
9th, base material heating-up temperature is 80 DEG C；
10th, crucible heating-up temperature is 400 °, and heating-up temperature has no problem, upper and lower temperature difference ± 5 DEG C；
11st, the crucible heat time is 22min；
12nd, crucible cool time is 31min；
13rd, temperature is 46 DEG C after crucible cooling；
14th, home roll rotating speed is 16m/min, and home roll speed can make adjustment according to needs during plated film, scope 6m/min~
80m/min；
15th, home roll temperature is 70 DEG C~80 DEG C, and the source of home roll temperature is that evaporator crucible heating and evaporation process are received and absorbed
The heat arrived；
16th, X-ray thickness gauges 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%；
17th, epicoele venting duration is 8min；
18th, cavity of resorption venting duration is 10min；
19th, base material chilling temperature is 31 DEG C, sets temperature-detecting device after evaporation, and detection base material is cooled down by chill roll 6
Temperature estimate value should be in the range of 100~150 DEG C after actual temperature afterwards, evaporation.By the cooling rear substrate cooling temperature of chill roll 6
Spend for 31 DEG C.
20th, base material cool time is 5s；
21st, evaporation time is 28min；
22nd, evaporation thickness is 10 μm, and evaporation starts that head thickness is relatively low probably has 5m or so, is adjusted tape running speed
Afterwards, between qualified 9.4 μm~10.5 μm of thickness range；
23rd, coating uniformity is detected as within ± 10%；Time detecting thickness deviation ± 5% or so；
24th, evaporation length is 400m；
25th, lithium metal utilization rate is 90.6%, 2kg lithium metals, and remaining 0.2kg, evaporation weight is 1.63kg, consumption
0.17kg。
Claims (10)
1. high-speed and continuous type vacuum vapor deposition lithium equipment, it is characterised in that high-speed and continuous type vacuum vapor deposition lithium equipment includes
Body fuselage (1), cavity dam (2), unreel system (3), substrate heater (4), home roll (5), chill roll (6), winding system
(7), crucible (8), crucible fixed mount (9), crucible heater (10), heat-insulation 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
The visual windows that feed (18)；
High-speed and continuous type vacuum vapor deposition lithium equipment is separated into upper cavity with by cavity dam (2) and body fuselage (1)
Cavity, system (3), substrate heater (4), chill roll (6) and the winding system (7) of unreeling is arranged on high-speed and continuous takeup type
In the upper cavity of vacuum evaporation lithium equipment, it is described unreel transition roller (13) be arranged on the system of unreeling (3) and substrate heater (4) it
Between, the heating transition roller (14) is arranged between home roll (5) and substrate heater (4), and the cooling transition roller (15) is set
Between home roll (5) and chill roll (6)；The crucible (8), crucible fixed mount (9), crucible heater (10), heat-insulation layer (11)
In the lower chamber that high-speed and continuous type vacuum vapor deposition lithium equipment is arranged on crucible lifting-transverse shifting platform (12), the crucible is consolidated
Determine frame (9) to be fixedly connected with body fuselage (1) inwall, the heat-insulation layer (11) is arranged on crucible lifting-transverse shifting platform (12),
It is used to be incubated using heat-insulation layer (11) cladding crucible heater (10), the crucible (8) is carried on crucible fixed mount (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
OK；Epicoele vacuum valve (16) is set on epicoele body sidewall, cavity of resorption vacuum valve (17) is set in lower chamber side wall upper part,
Lower chamber top side wall sets charging visual windows (18)；The home roll (5) passes through cavity dam (2), and a part is in epicoele
In body, another part is in lower chamber, and the distance of home roll (5) and cavity dam (2) is 5mm~10mm；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes coating detecting system, detects cold using coating detecting system
But roller (6) and cooling transition roller (15) and between substrate surface coating thickness；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes pumped vacuum systems, using pumped vacuum systems to high-speed and continuous
The upper cavity and lower chamber of type vacuum vapor deposition lithium equipment carry out vacuumize process；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes PLC control system, is controlled at a high speed using PLC control system
Continuous type vacuum vapor deposition lithium equipment running；
The high-speed and continuous type vacuum vapor deposition lithium equipment also includes crucible cooling system, and the crucible cooling system is comprising cold
But oil, crucible controllable silicon and crucible cooler, the side wall of the crucible fixed mount (9) is hollow structure, and cooling oil is loaded in earthenware
In the hollow structure of crucible fixed mount (9) side wall, oil cooling is carried out to crucible (8) using cooling oil, crucible controllable silicon and crucible is utilized
Cooler carries out circulating cooling to cooling oil.
2. high-speed and continuous type vacuum vapor deposition lithium equipment according to claim 1, it is characterised in that described to unreel system
Include let off roll, deviation-rectifying system, transition roller system, base material evaporation rate control system, tension control system and flattening system.
3. high-speed and continuous type vacuum vapor deposition lithium equipment according to claim 1, it is characterised in that the winding system
Include wind-up roll, mechanical expansion shaft, AC driven motor, frequency-variable controller, SKF bearings, magnet fluid sealing and feeding turntable.
4. high-speed and continuous type vacuum vapor deposition lithium equipment according to claim 1, it is characterised in that on the home roll (5)
Temperature transmitter and home roll controllable silicon are set.
5. high-speed and continuous type vacuum vapor deposition lithium equipment according to claim 1, it is characterised in that the chill roll (6)
Connect controllable silicon and cooler.
6. high-speed and continuous type vacuum vapor deposition lithium equipment according to claim 1, it is characterised in that the body fuselage
(1) material is stainless steel, thickness 50mm.
7. high-speed and continuous type vacuum vapor deposition lithium equipment according to claim 1, it is characterised in that the crucible (8) is
Semicircle or rectangle；And the diameter ratio of the width of the crucible (8) and home roll (5) is 1:(3~10).
8. the method that lithium is deposited in base material is realized using the high-speed and continuous type vacuum vapor deposition lithium equipment described in claim 1, its
It is characterized by high-speed and continuous type vacuum vapor deposition lithium equipment and realizes that the method for base material evaporation lithium is to complete according to the following steps
's：
First, the preparatory stage：1., by base material be worn in high-speed and continuous type vacuum vapor deposition lithium equipment after closure upper cavity and under
Cavity, 2., by lithium metal adds in crucible (8) along charging visual windows (18), crucible (8) then is moved into crucible heater
(10) on, and crucible (8) puts, adjustment crucible lifting-transverse shifting platform (12) consistent with home roll direction, makes crucible (8) and home roll
(5) distance of surface substrate is 5mm~20mm, 3., to high-speed and continuous type vacuum vapor deposition lithium equipment is sealed；
2nd, vacuumize：The upper cavity of high-speed and continuous type vacuum vapor deposition lithium equipment is vacuumized, the vacuum to upper cavity is
6.5×10-2Pa~7 × 10-2Untill Pa, while being vacuumized to the lower chamber of high-speed and continuous type vacuum vapor deposition lithium equipment, extremely
The vacuum of lower chambers is 7 × 10-3Pa~7 × 10-4Untill Pa；
3rd, it is deposited：Start crucible heater (10), and detect crucible (8) interior lithium metal temperature in real time, when crucible (8) interior metal
When lithium temperature reaches 350 DEG C, startup unreels system (3), substrate heater (4) and winding system (7), adjustment high-speed and continuous winding
Formula vacuum evaporation lithium equipment operational factor, untill substrate surface lithium layer thickness reaches actual requirement, and in current operating parameter
Under the conditions of to ensure that high-speed and continuous type vacuum vapor deposition lithium equipment is carried out normal；
4th, pressure release is cooled down：Complete after base material evaporation lithium, closing crucible heater (10), unreel system (3), substrate heater (4)
With winding system (7), crucible (8) is moved on crucible fixed mount (9), using oil by adjustment crucible lifting-transverse shifting platform (12)
Crucible (8) is cooled to 40~50 DEG C by cold mode, now releases the vacuum pressure of upper cavity and lower chamber；
5th, base material is taken：The upper cavity and lower chamber of high-speed and continuous type vacuum vapor deposition lithium equipment are opened, surface evaporation lithium is taken out
Base material.
9. utilization high-speed and continuous type vacuum vapor deposition lithium equipment according to claim 8 realizes that the side of lithium is deposited in base material
Method, it is characterised in that temperature transmitter and home roll are set on the home roll (5) of the high-speed and continuous type vacuum vapor deposition lithium equipment
Controllable silicon, using temperature transmitter and home roll controllable silicon by the temperature control of home roll (5) surface substrate below 80 °；The height
Chill roll (6) the connection controllable silicon and cooler of fast continuous type vacuum vapor deposition lithium equipment, will using controllable silicon and cooler
Chill roll (6) temperature control is 10 DEG C~20 DEG C.
10. utilization high-speed and continuous type vacuum vapor deposition lithium equipment according to claim 8 realizes that the side of lithium is deposited in base material
Method, it is characterised in that step one 1. described in base material wearing concrete operations it is as follows：Base material is first rolled up into unreeling in the system that unreels (3)
On roller, then base material is sequentially passed through and unreels transition roller (13), it is 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), that is, complete base material 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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| CN107177820B CN107177820B (en) | 2019-05-24 |
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| CN108517509A (en) * | 2018-04-24 | 2018-09-11 | 广州市邦图机电科技有限公司 | A kind of application method of high vacuum takeup type capacitance coating machine |
| CN109402589A (en) * | 2019-01-02 | 2019-03-01 | 重庆天齐锂业有限责任公司 | A kind of magnetron sputtering prepares the method and system of super thin metal lithium film |
| CN109778135A (en) * | 2019-03-28 | 2019-05-21 | 中国科学院青岛生物能源与过程研究所 | A kind of pre- insertion lithium metal prepares the device and method of cell negative electrode material |
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| CN111430659A (en) * | 2019-11-27 | 2020-07-17 | 蜂巢能源科技有限公司 | Pre-lithiation treatment method for lithium ion battery cathode, lithium ion battery cathode and lithium ion battery |
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| 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 |
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