EP3559304A1 - Lineare dampfquelle - Google Patents

Lineare dampfquelle

Info

Publication number
EP3559304A1
EP3559304A1 EP17816650.0A EP17816650A EP3559304A1 EP 3559304 A1 EP3559304 A1 EP 3559304A1 EP 17816650 A EP17816650 A EP 17816650A EP 3559304 A1 EP3559304 A1 EP 3559304A1
Authority
EP
European Patent Office
Prior art keywords
crucible
nozzle
roll
evaporated
evaporation source
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP17816650.0A
Other languages
English (en)
French (fr)
Inventor
Marc Kaelin
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Flisom AG
Original Assignee
Flisom AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Flisom AG filed Critical Flisom AG
Publication of EP3559304A1 publication Critical patent/EP3559304A1/de
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/243—Crucibles for source material
    • 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

Definitions

  • the present invention relates to linear evaporation sources used for vapor deposition of material onto substrates and more particularly for controlled material coating of large substrates, such as vacuum deposition on large sheets or using roll-to-roll processes.
  • the present invention relates to linear evaporation sources usable for vapor deposition of In, Ga and Cu for controlled material coating of large flexible substrates in vacuum using the roll-to-roll process for the production of thin films of CIGS (Cu(ln,Ga)Se2, copper indium gallium di selenide).
  • CIGS thin film means a CIGS film exhibiting a thickness between 50 and 0.1 micrometers, most preferably between 5 and 0.5 micrometers.
  • a further problem in the field of thermal vapor deposition during long deposition cycles relates to the falling of material flakes or other particles into the evaporation source. It is therefore also an object of the current invention to provide an evaporation source that prevents problems associated with falling material flakes.
  • high output evaporation source means an evaporation source capable to depose per unitary length a material flux higher than 5 nm cm/s, preferably higher than 100 nm cm/s, most preferably higher than 150 nm cm/s, so as to be suited to coat large webs and foils in an industrial roll-to-roll manufacturing coating step with acceptable speed.
  • said at least one nozzle is inclined, and has a flux-wise axis that is oriented at between +30 degrees and +80 degrees with respect to the plane supporting the base of at least one nozzle, preferably between +40 and +70 degrees, most preferably between +45 and +60 degrees, so as to direct the evaporated flux away from the orthogonal to said base.
  • said at least one nozzle exhibits a channel having a flux-wise axis, said channel exhibiting a length longer than its width, preferably longer than two times its width, more preferably longer than three times its width, and exhibits a divergent cross section, i.e. a cross-section along a plane containing the flux- wise axis larger at the nozzle outlet than at the nozzle inlet, so as to be configured to convey the evaporated material on the largest possible surface of the adjacent thin web.
  • the web may exhibit different slopes and orientations in respect to the ground, and the at least three evaporation source apparatuses may exhibit nozzles having a flux-wise axis always oriented perpendicularly to the adjacent surface of the web, so as to direct always the evaporated flux orthogonally to the adjacent surface of the web.
  • Another aspect of the invention is a method for the deposition of thin CIGS films on a thin web with a roll-to roll vapor deposition system, comprising a vacuum deposition chamber enclosing at least three evaporation source apparatuses according to the invention, containing respectively In, Ga and Cu, characterized in that the web, for example made of polymer or metal foil, departs a pay-off roll, gets coated with a thin CIGS film by said evaporation sources as it travels between tensioning rolls until it gets rolled-up by take-up roll .
  • At least one heating element is an electrically heatable rod or an electrically heatable coil, in both cases made of an electrically-conductive and heat-resistant material, in particular tantalum, graphite, tungsten, or molybdenum.
  • the apparatus can further comprise at least one heat shield assembly that at least partially surrounds the crucible.
  • at least one heat shield assembly that at least partially surrounds the crucible.
  • an external opening of a nozzle can protrude through and beyond the thickness of the heat shield assembly adjacent to the nozzle, so as to avoid a deposition of the evaporated atoms onto the external surface of the crucible or lid.
  • at least one lip pair can join the crucible with a lid such that said lip pair extends through the heat shield assembly and is equal or greater than the total thickness of the heat shield assembly at the edge of the lip pair, so as to avoid a deposition of the evaporated atoms onto the external surface of the shield, or crucible or lid.
  • the nozzles positioned above the level of material to be evaporated advantageously reduce the evaporation source's volume and keep the material hot at the surface where evaporation occurs, thereby permitting a faster response to changes in temperature of the heating elements and subsequent energy savings.
  • the nozzles advantageously help to solve the problem of uneven spatial distribution of the deposited material and reduce energy expense to obtain a uniform deposition profile.
  • the at least one heat shield assembly that at least partially surrounds the crucible advantageously insulates the source and therefore reduces the amount of heat radiated to adjacent objects.
  • the external opening of the nozzles protruding through and beyond the thickness of the heat shield assembly advantageously reduces the possibility of material depositing onto the shields.
  • the exemplary embodiments presented in this disclosure show an evaporation source comprising a crucible, itself comprising at least three heating elements, at least one of which is contained within said crucible.
  • the crucible is ordinarily closed by a lid.
  • the heating element located within the crucible is positioned close to the top of the crucible and close to nozzle orifices present either in the lid or near the top of one of the crucible's long walls.
  • Said nozzles may be shaped/oriented so as to direct the vapor flux in a desired direction. This proximity of the inner heating element to the nozzles ensures firstly that the heating elements block the line of sight from outside the evaporation source through the nozzles towards the material to be evaporated, and secondly that the nozzles are heated.
  • FIG. 1 B shows a preferred embodiment of the evaporation source 200 of FIG. 1A where crucible 50 is closed by lid 60.
  • Crucible 50 and lid 60 are ordinarily made of a refractory material for example primarily containing alumina (AI2O3), silica, boron nitride, graphite, molybdenum, tantalum, or tungsten.
  • Lid 60 comprises at least one nozzle 65 positioned over heater assembly 100.
  • Lid 60 preferably comprises a plurality of nozzles 65 wherein no nozzle 65 provides a line of sight from outside crucible 50 to the surface of the material to be evaporated contained within crucible 50.
  • Temperature sensor 71 is also present in the cross-section of the crucible bottom. Hole 52 serves in this embodiment as a channel for temperature sensor 72 in case there is a need to measure temperatures closer to the mid-length of crucible 50.
  • FIG. 1 C illustrates how the channel of nozzle 65 may be designed so as to direct the evaporated flux at an angle that is not orthogonal to the plane of lid 60. The angle at which nozzle 65 is oriented will ordinarily be between +30° and +150° with respect to the plane onto which nozzle 65 is fitted, in the present case the plane of lid 60.
  • FIG. 1 C also shows how crucible 50 and lid 60 are provided with respective extended lips 56, 66 at the perimeter where they are in contact. The pair of lips 56, 66 acts as a circumferential joint which may also channel the vapor flux of material 55 that may leak through the pair of lips 56, 66 between crucible 50 and lid 60.
  • Said lips 56, 66 help reduce the amount of material that may deposit on an optional heat shield assembly presented in FIGS.1 D-1 E.
  • FIG. 2A shows an assembly of three axially aligned electrical heating coils 10, 20, 30.
  • the central heating coil 10 is powered at each of its extremities via extended insulated contacts 1 1 , 12.
  • Insulated contacts 1 1 , 12 are located close to the common axis of heating coils 10, 20, 30 and extend in a direction parallel to said common axis.
  • Heating coil 20 is located at one of the extremities of heating coil 10 and surrounds insulated contact 1 1.
  • Heating coil 30 is located at the other extremity of heating coil 10 and surrounds insulated contact 12.
  • Heating coils 20 and 30 are powered via insulated contacts 21 , 22 and 31 , 32, respectively.
  • FIG. 2D shows an embodiment of an evaporation source 200 comprising a crucible 50, ordinarily an elongated container of trapezoidal cross-section made of refractory material, and a heater assembly 100 aligned with the crucible's long centerline and passing through corresponding holes in each trapezoid short side.
  • Heater tube 40 is positioned close to the crucible's opening or top so that the material to be evaporated, also called a melt, remains at the crucible's bottom and below heater tube 40 during ordinary operation.
  • Evaporation source 200 further comprises at least three temperature sensors 71 , 72, 73, such as thermocouples, positioned against the part of crucible 50 containing said melt.
  • Heating rods 8, 9, 10 are electrically connected in parallel so as to represent a single heating element and powered via insulated contacts 1 1 , 12.
  • Heating rods 8, 9, 10 may also be connected in series or any combination of parallel and series, or that the number of heating rods positioned within crucible 50 and close to its top may be increased.
  • Heating assembly 100 further comprises side heaters 20 and 30 that are mounted outside crucible 50 against each short face and powered by contacts 21 , 22 and 31 , 32, respectively. It is understood that if the crucible 50 is surrounded by heat shields as in Figs. 1 D and 1 E, the side heaters 20 and 30 will be located inside the heat shields. Similarly to crucibles 50 of embodiments presented in FIGS.
  • FIG. 4B shows a cross-section of the embodiment of evaporation source 200 of FIG. 4A. It is conceptually similar to the cross-section of FIG. 1 C with a crucible 50 containing molten material to be evaporated 55 at its bottom and comprising temperature sensor 71 , temperature sensor channel 52, three parallel heating rods 8, 9, 10, and lid 60 bearing nozzles 65.
  • FIG. 4B details how the walls of crucible 50 differ from that of FIG. 1 C: the shape of crucible 50 is modified to support lid 60 bearing side-facing nozzles 65.
  • FIG. 4B also shows that the line of sight from outside evaporation source 200 through nozzles 65 towards the material to be evaporated 55 is obstructed by heating rod 9.
  • FIG. 4D shows a cross-section of the embodiment of evaporation source 200 of FIG. 4C. It is conceptually similar to the cross-section of FIG. 1 C with a crucible 50 containing molten material to be evaporated 55 at its bottom and comprising temperature sensor 71 , temperature sensor channel 52, three parallel heating rods 8, 9, 10, and a lid 60 that bears no nozzles. In this embodiment, it is crucible 50 that bears convergent-divergent nozzles 65 close to the top of one of its side walls that runs parallel to heating rod 9.
  • FIG. 4D also shows that the line of sight from outside evaporation source 200 through nozzles 65 towards the material to be evaporated 55 is obstructed by heating rod 9.
  • a first advantage results from the use of nozzles able to direct the evaporated flux in a predetermined direction along the evaporation source's length to solve the problem of uneven spatial distribution of the deposited material.
  • Deposition with conventional crucibles ordinarily exhibits a decay of evaporated material deposition profile towards the extremities of the crucible's long axis. The decay is ordinarily compensated for a set point by supplying more heat to the crucible.
  • the benefit of using nozzles able to direct the evaporated flux in a predetermined direction is that the resulting deposition profile is more uniform at less energy expense while being easily adaptable via regulation of the independent power supplies.
  • a further advantage of this disclosure is that the heat needed to produce a desired deposition profile can be tuned as the material to be evaporated depletes within the evaporation source or as the heat shields experience changes in their properties. Independent adjustments of the heat produced by the heating elements therefore regulate the evaporation profile. Furthermore, said adjustments prevent the onset of unwanted vapor flow along the crucible's long axis.
  • the ability to continuously regulate the evaporation profile is especially beneficial for vapor deposition onto large substrates, for example roll-to-roll webs 0.5 meters wide or more, or also glass substrates larger than 0.5 meters in width or length. It then becomes possible to advantageously integrate an evaporation sources feedback control function as part of an evaporation source system. Said feedback control function would at least use temperatures measured by the evaporation source's temperature sensors and possibly also measurements of the material deposited onto the substrate.
  • FIG. 6B therefore presents an advantageous cabling solution to electrically connect heating elements to power supplies.
  • using shared power lines may, under some conditions, enable to reduce the electrical current flowing through some of the lines, thereby further simplifying the cabling between heating elements and power supplies.
  • placing the heating assembly mainly within the crucible rather than outside is beneficial to reduce the evaporation source's volume. This is especially advantageous for use within vacuum deposition chambers where several evaporation sources might be used within a restricted volume. For example in the context of a co-evaporation vacuum deposition chamber, it is advantageous to have evaporation sources arranged in parallel and close to each other. Also, the coaxial configuration of the heating assembly presented in the embodiments of FIGS. 1 and 2 reduces the complexity of external wiring needed to power the heating elements in comparison to configurations found in prior art. Benefits of this reduction in wiring are increased overall reliability and reduction of assembly cost.
  • a roll-to roll vapor deposition system 800 was actually built for the deposition of thin CIGS films on a thin web (830), comprising a vacuum deposition chamber (810) enclosing at least three evaporation sources (822, 823, 824) according to the invention, containing respectively In, Ga and Cu, whereby web (830), made of polyimide foil, departs a pay-off roll (841 ) and gets coated by said evaporation sources (822, 823, 824) as it travels between tensioning rolls (851 , 852, 853, 854) until it gets rolled-up by take-up roll (842).

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
EP17816650.0A 2016-12-22 2017-12-07 Lineare dampfquelle Pending EP3559304A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP16206164 2016-12-22
PCT/EP2017/081925 WO2018114377A1 (en) 2016-12-22 2017-12-07 Linear vapor source

Publications (1)

Publication Number Publication Date
EP3559304A1 true EP3559304A1 (de) 2019-10-30

Family

ID=57629381

Family Applications (1)

Application Number Title Priority Date Filing Date
EP17816650.0A Pending EP3559304A1 (de) 2016-12-22 2017-12-07 Lineare dampfquelle

Country Status (2)

Country Link
EP (1) EP3559304A1 (de)
WO (1) WO2018114377A1 (de)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113227436A (zh) * 2018-12-21 2021-08-06 应用材料公司 气相沉积装置和用于在真空腔室中涂布基板的方法
CN111485201B (zh) * 2019-01-28 2024-05-24 广州先艺电子科技有限公司 一种真空蒸镀设备的蒸发源
DE102021117576B4 (de) * 2021-07-07 2023-02-09 Thyssenkrupp Steel Europe Ag Beschichtungsanlage zur Beschichtung eines Gegenstands

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Publication number Priority date Publication date Assignee Title
GB554312A (en) 1941-12-26 1943-06-29 Zoltan Deshaw Improvements in and relating to the separation of metal parts cemented together by corrosion
US2440135A (en) 1944-08-04 1948-04-20 Alexander Paul Method of and apparatus for depositing substances by thermal evaporation in vacuum chambers
US20010005553A1 (en) * 1999-11-10 2001-06-28 Witzman Matthew R. Linear aperture deposition apparatus and coating process
EP1496134B1 (de) * 2003-07-04 2015-03-25 Agfa HealthCare NV Gerät zur Dampfabscheidung
ATE364098T1 (de) 2004-11-20 2007-06-15 Applied Materials Gmbh & Co Kg Vorrichtung zum verdampfen von materialien
JP2006225757A (ja) 2005-01-21 2006-08-31 Mitsubishi Heavy Ind Ltd 真空蒸着装置
JP2007186787A (ja) * 2005-12-14 2007-07-26 Hitachi Displays Ltd 蒸着坩堝並びにこれを備えた薄膜形成装置、及び表示装置の製造方法
WO2009033503A1 (en) 2007-09-12 2009-03-19 Flisom Ag Method for manufacturing a compound film
TW201122128A (en) * 2009-12-31 2011-07-01 Axuntek Solar Energy Co Ltd Evaporation source device (I)
EP2577732B1 (de) 2010-05-28 2019-03-13 Flisom AG Verfahren und vorrichtung für ein dünnschichtmodul mit gepunkteten vernetzungen und durchgängen
JP5465136B2 (ja) * 2010-08-31 2014-04-09 富士フイルム株式会社 蒸着フラックス測定装置および真空蒸着装置
JP5520871B2 (ja) * 2011-03-31 2014-06-11 株式会社日立ハイテクノロジーズ 蒸着装置
TWI538235B (zh) 2011-04-19 2016-06-11 弗里松股份有限公司 薄膜光伏打裝置及製造方法
TWI654771B (zh) 2012-12-21 2019-03-21 瑞士商弗里松股份有限公司 附加著鉀之薄膜光電裝置的製造
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Also Published As

Publication number Publication date
WO2018114377A1 (en) 2018-06-28

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