• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The present invention relates to a method of reloading an evaporation cell (10) for evaporating a material (7) on a substrate placed in a vacuum deposition chamber, a first crucible (110) containing the material to be evaporated being engaged with an evaporation chamber (100) of the evaporation cell, and evaporation means (101, 131, 132) being provided to bring the first crucible into evaporation conditions to generate a vapor flow (116). ) of the material. This recharging process comprises a step of loading a second crucible (120) containing the material to be evaporated in a charging chamber (200) previously isolated from the adjoining evaporation chamber, the pressure in the charging chamber then being substantially greater than that in the vacuum deposition chamber; a confinement step for reducing the pressure inside the charging chamber to a level comparable to that of the evaporation chamber during the evaporation of the first crucible; a release step in which the first crucible is transferred to the charging chamber, a step of engagement of the second crucible with the evaporation chamber, and a step of setting evaporation conditions of the second crucible.
    公开号:FR3018082A1
    申请号:FR1451712
    申请日:2014-03-03
    公开日:2015-09-04
    发明作者:David Esteve；Franck Stemmelen；Oliveira Christophe De
    申请人:Riber SA；
    IPC主号:
    专利说明:

    [0001] The invention relates to the field of evaporation and vacuum deposition of materials on a substrate. The invention more particularly relates to a method of reloading an evaporation cell for evaporating a material for deposit on a substrate placed in a vacuum deposition chamber. A vacuum deposition apparatus makes it possible to deposit a material, such as a semiconductor material or compound (for example: silicon, gallium arsenide, indium phosphide, etc.), an inorganic material (for example: selenium, antimony, phosphorus), or an organic material (for example: tris (8-hydroxyquinoline) aluminum (III) or Alq 3,...), evaporated in an evaporation chamber, on a substrate placed in a deposition chamber maintained under vacuum. Such an apparatus comprises in particular an evaporation cell for evaporating the material, a first crucible containing the material to be evaporated then being engaged with the evaporation chamber of said evaporation cell, evaporation means being provided for to put this first crucible in evaporation conditions to generate a flow of vapor of the material through an outlet orifice of the evaporation chamber, the outlet orifice being connected to an injector for the injection of steam into the vacuum deposition chamber. To ensure almost continuous production, an evaporation cell can be operated using a large capacity crucible containing a large amount of material to be evaporated, so that it is then possible to deposit the material on a large number of successive substrates. . However, using high capacity crucibles, it is necessary during their replacement to wait for their cooling before being able to recharge the evaporation cell so that the thermal stability of the evaporation chamber is not disturbed by the withdrawal. of a hot crucible and the introduction of a cold crucible into the evaporation chamber. Thus, the refilling of the evaporation cell leads to a long interruption of production, a new crucible can not be prepared for its evaporation before having been able to release the first crucible of the evaporation cell. This interruption of production, which can range from a few hours to several days depending on the size of the crucibles, reduces the production yield and increases the cost of the deposition operation of the material on the substrate. In order to overcome the above-mentioned disadvantage of the state of the art, the present invention proposes a method of reloading an evaporation cell making it possible to reduce or even eliminate the interruption times of a method of deposition implemented by a vacuum deposition apparatus using this evaporation cell. To this end, the invention relates to a method of reloading an evaporation cell for evaporating a material for depositing it on a substrate placed in a deposition chamber maintained under vacuum, a first crucible containing said material to be evaporated. being engaged with an evaporation chamber of said evaporation cell, evaporation means being provided for putting said first crucible in evaporation conditions to generate a flow of vapor of the material through an outlet orifice of said evaporation chamber, said outlet orifice being connected to an injector for injecting said vapor into said vacuum deposition chamber, said recharging method comprising: a step of loading a second crucible containing the material to be evaporated in a loading chamber previously isolated from said adjoining evaporation chamber, the pressure in said loading chamber then being substantially greater than that prevailing in the vacuum deposition chamber, - after said introduction step, a step of confining said loading chamber intended to reduce the pressure inside said charging chamber to a level comparable to that of said evaporation chamber during the evaporation of said first crucible, - after said confinement step, a step of releasing said first crucible from said evaporation chamber in which said first crucible is transferred from said chamber of said evaporation towards said loading chamber, - after said step of releasing the first crucible, a step of engagement of said second crucible with said evaporation chamber, and after said step of engaging said second crucible, a step of bringing into effect evaporation of said second crucible to generate a vapor flow of the material through said outlet orifice of the evaporator chamber tion. The reloading method according to the invention therefore makes it possible to rapidly change the crucible without long interruption of the deposition process.
    [0002] Indeed, thanks to said loading chamber previously isolated from said evaporation chamber, it is possible, before the first crucible release step, to prepare the second crucible while the first crucible is being evaporated in the first crucible. evaporation cell. The reloading process is particularly suitable in the case where small crucibles are used which require frequent crucible replacement. Furthermore, other advantageous and non-limiting characteristics of the process according to the invention are the following: during said step of engagement of said second crucible, said loading chamber is isolated from said evaporation chamber and said vacuum deposition chamber; during said step of loading said second crucible, an access hatch of said loading chamber is opened and said second crucible is introduced from the outside of said evaporation cell into said loading chamber; through said access hatch; during said confinement step, said access hatch is closed in leaktight manner with respect to the outside of said evaporation cell, and pumping is carried out inside said loading chamber; during said step of releasing the first crucible, said first crucible is removed from said evaporation chamber by passing it through an insertion opening communicating said loading chamber and said evaporation chamber, and during said step of engaging said second crucible, said second crucible is inserted into said evaporation chamber by passing it through said insertion opening, and said insertion opening is closed in a sealed manner to isolate said chamber loading said evaporation chamber; said recharging process comprises, prior to said step of engagement of said second crucible with said evaporation chamber, a step of preparation of said second crucible in said loading chamber intended to reduce the duration of said step of bringing into being of evaporation conditions of said second crucible; - said preparation step comprises a step of preheating said second crucible in said charging chamber, to a predetermined preheating temperature.
    [0003] Embodiments of the invention will be described in detail with reference to the drawings in which: - Figure 1 is a schematic overall sectional view in a vertical plane of a vacuum deposition apparatus according to an embodiment of the invention comprising an evaporation cell and a vacuum deposition chamber; Figure 2A is a schematic sectional view in a vertical plane of a first example of an evaporation cell having an evaporation chamber with which a first solid crucible is engaged, and an adjoining charging chamber comprising an empty crucible; Fig. 2B is a detail view of area ii of Fig. 2A; FIG. 3 is a diagrammatic sectional view in a vertical plane of the evaporation cell of FIG. 2A during the initial loading of the loading chamber with a second solid crucible; - Figure 4 is a schematic sectional view in a vertical plane of the evaporation cell of Figure 2A during the evaporation of the first crucible; - Figure 5 is a schematic sectional view in a vertical plane of the evaporation cell of Figure 2A before release of the first empty crucible with the evaporation chamber; Figure 6 is a schematic sectional view in a vertical plane of the evaporation cell of Figure 2A after release of the first empty crucible from the evaporation chamber; Figure 7 is a schematic sectional view in a vertical plane of the evaporation cell of Figure 2A before engagement of the second solid crucible with the evaporation chamber; Figure 8 is a schematic sectional view in a vertical plane of the evaporation cell of Figure 2A after engagement of the second crucible with the evaporation chamber, during the step of conditioning the second crucible; Figure 9A is a schematic sectional view in a vertical plane of a second example of an evaporation cell; FIG. 9B is a detailed view of zone IX of FIG. 9A showing the means for closing an insertion opening between the evaporation chamber and the loading chamber of the evaporation cell of FIG. 9A. ; Figure 10 is a schematic view of a third example of an evaporation cell having a sealed valve between the evaporation chamber and the injector; Figure 11 is a schematic view of a variant of the third example of the evaporation cell of Figure 10 wherein the outer chamber of the evaporation chamber is isolated from the vacuum deposition chamber; Figure 12 is a schematic view of a fourth example of an evaporation cell having two separate evaporation chambers. In the following description, the terms "up" and "down" will be used by reference to the vertical, relative to the room in which the vacuum deposition apparatus is installed, the top designating the side facing the ceiling of the local and the bottom designating the side facing the floor. Similarly, the terms "lower" and "upper" will refer to the sides turned downward and upward respectively. FIG. 1 is a diagrammatic overall view in section in a vertical plane of a vacuum deposition apparatus 1 which comprises, on the one hand, an evaporation cell 10, and, on the other hand, a vacuum deposition chamber 20.
    [0004] In general, the evaporation cell 10 of the vacuum deposition apparatus 1 is intended to evaporate a material for depositing it on a substrate 2 placed in the vacuum deposition chamber 20, here in a lower part 23. of it. It will be seen in the following description that the evaporation cell 10 is designed to generate an upstream vapor stream 3 of said material, upstream vapor stream 3 which is transported by an injection conduit 14 from the evaporation cell 10 to an injector 13 located in the upper part 22 of the vacuum deposition chamber 20. The evaporation cell 10 and the vacuum deposition chamber 20 are connected to each other by a tubular connection 5 crossed by the injection conduit 14.
    [0005] The injector 13 of the evaporation cell 10 injects the vapor of material transported by the injection duct 14 into the vacuum deposition chamber 20 according to a downstream vapor flow 4 directed downwards towards the substrate 2, so that the material is deposited on an upper face 2A of the substrate 2 facing the injector 13.
    [0006] The injector 13 is designed to optimize the characteristics of the downstream vapor flow 4 directed towards the substrate 2, for example its flow rate or its spatial distribution, so that the layer of material deposited on the upper face 2A of the substrate 2 has the properties required such as thickness, surface condition, conductivity, etc., depending on the intended application.
    [0007] There is provided inside the injector 13 specific heating means (not shown) for preventing the condensation of material vapors inside the injector 13, which could compromise its proper operation. In order to realize and maintain the vacuum inside the vacuum deposition chamber 20, the vacuum deposition apparatus 1 comprises pumping means 6 connected to the vacuum deposition chamber 20 whose pumping capacities are adjusted to the internal volume 29 of the vacuum deposition chamber 20. These pumping means 6 here comprise a turbo-molecular pump or a cryogenic pump which lower the pressure level prevailing inside the deposition chamber under vacuum 20 to 10-3 at 10-8 Torr.
    [0008] A first example of an evaporation cell 10 intended to produce a downstream vapor stream 3 towards the injector 13 will now be described with reference to FIGS. 2 to 9B. A reloading process according to the invention will also be described. to operate this evaporation cell 10 almost continuously, that is to say by limiting the downtime of the production of the downstream vapor stream 3.
    [0009] As shown in FIG. 2A, the evaporation cell 10 of the vacuum deposition apparatus 1 firstly comprises an external enclosure 11, here of generally cylindrical shape, comprising a side wall 11A, an upper wall 11B ( or "roof"), and a bottom wall 11C (or "bottom"). It is provided on the internal faces of the side wall 11A and the upper wall 11B of the outer enclosure 11, and also the tubular connector 5, heating elements, for example heating resistors 16, for heating in a substantially homogeneous the internal volume 19 of the outer enclosure 11, in particular the injection conduit 14, so as to prevent the material vapors from condensing on cold parts of the evaporation cell 10.
    [0010] It is also provided, this time on the outer faces of the side wall 11A, the upper wall 11B, and also the tubular connector 5, cooling elements (not shown), for example cold water coils, so that the outer enclosure 11 of the evaporation cell 10 is cold to the touch from the outside.
    [0011] Between the heating elements 16 and the cooling elements is inserted a radiative screen, for example made in the form of a refractory material, so that the heating and cooling are effective each on their side. The side wall 11A comprises an opening 11D from which extends outwardly the tubular connector 5 for the connection of the evaporation cell 10 to the vacuum deposition chamber 20 of the vacuum deposition apparatus 1. In this configuration (common to Figures 1 to 10 and 12), the outer enclosure 11 and the vacuum deposition chamber 20 are in communication and share the same vacuum so that when the vacuum is made inside the chamber vacuum deposition 20, it is also made inside the outer enclosure 11 of the evaporation cell 10. The pressure level in this outer chamber 11 is thus equal to that prevailing in the vacuum deposition chamber 20. Alternatively, as shown in FIG. 11, it is possible to provide a tight seal 18 between the tubular connection 5 and the injection duct 14 of the evaporation cell 10, so that the outer enclosure 11 of the cell Evaporation 10 does not share the same In this case, the evaporation cell 10 then comprises an enclosure pump 19A which is dedicated thereto and which is intended to pump the internal volume 19 of the external enclosure 11 to reduce the pressure to a level of 10-2 to 10-3 Torr. As can be seen in FIGS. 2A and 2B, an opening, hereinafter referred to as the insertion aperture 12, is cut in the bottom wall 11C of the outer enclosure 11. This insertion opening 12 has an inner edge 12A, which is here of circular shape, above which extends, towards the inside of the outer enclosure 11, an evaporation chamber 100 of the evaporation cell 10. This evaporation chamber 100 is delimited by a sealed wall comprising, on the one hand, a cylindrical body 101 coaxial with the insertion opening 12, and, on the other hand, a frustoconical collar 102 extending the body 101, to an outlet orifice 103 of the chamber 100. This body 101 of the evaporation chamber 100 has a lower edge 101A which runs continuously along the inner edge 12A of the insertion opening 12. The lower edge 101A is hermetically fixed on the bottom wall 11C of the outer enclosure 11 of the cell 10 so that the internal volume 19 of the outer enclosure 11 of the evaporation cell 10 does not communicate with the internal volume 104 of the evaporation chamber 10. The outlet orifice 103 of the chamber Evaporation 100 is sealingly connected to the injection duct 14 of the evaporation cell 10 forming here a bend 14A at said outlet port 103. The sealed connection can be made, for example, by means of a weld .
    [0012] The evaporation chamber 100 of the evaporation cell 10 is intended to receive a crucible, such as the first crucible 110 (see FIG. 2A) and the second crucible 120 (see FIG. 3). These crucibles 110, 120 have shapes and dimensions adapted so that they can be housed in the evaporation chamber 100.
    [0013] Advantageously, the crucibles 110, 120 have a low volume capacity, less than 1 liter (L), preferably less than 0.5 L, for example equal to 0.33 L. They generally have the shape of a bottle and comprise a side wall 111, 121 which is closed downwards by a bottom 115, 125 and which narrows upwardly along a neck 112, 122 delimiting a neck 113, 123 of the crucible 110, 120.
    [0014] The crucibles 110, 120 are preferably made in one piece in a material having good infrared transparency and high temperature resistance. The crucibles 110, 120 may be, for example, made of a ceramic material such as pyrolytic boron nitride or PBN (for "Pyrolytic Boron Nitride" in English) or in a vitreous type material such as quartz.
    [0015] They are intended to be filled with the material 7 to be evaporated, this material 7 may be in liquid form, in powder form, or even in the form of ingots. When a crucible (case of the first crucible 110 in Figure 3, the case of the second crucible 120 in Figure 8) is engaged with the evaporation chamber, that is to say when it is housed inside the internal volume 104 of the evaporation chamber 100, its side wall 111, 121 is then found facing the body 101 of the evaporation chamber 100. In order to put in evaporation conditions a crucible 110, 120 engaged with the evaporation chamber 100, the evaporation cell also comprises evaporation means disposed at the periphery of the evaporation chamber 100 accommodating said crucible 110, 120. In all the examples described in FIGS. 2 to 12, these means the evaporation chamber 100 comprises, first of all, electrical resistances 131 surrounding the evaporation chamber 100 and extending from the bottom 11C of the outer enclosure 11, substantially parallel to the body 101 of the evaporation chamber 100, up to collar 102 thereof. These electrical resistors 131 are electrically powered and brought to high temperature so that they radiate heat, essentially in infra-red form.
    [0016] Alternatively, the evaporation means may comprise infrared lamps placed directly in the interior volume of the evaporation chamber, against the body thereof, so as to directly irradiate the crucible engaged in the evaporation chamber. The evaporation means also comprise a heat shield 132 located inside the outer enclosure 11 and interposed between the body 101 of the evaporation chamber 100 and the electrical resistors 131. As shown in FIG. 9B, this Thermal screen 132 is of the "telescopic" type and here comprises five cylindrical and coaxial movable elements 132A, 132B, 132C, 132D, 132E, which can fit into each other so that the height of the heat shield 132 can be adjusted to suit. For example, Figure 2A shows the heat shield 132 at its greatest height when all the movable members 132A, 132B, 132C, 132D, 132E are unfolded. Figure 6, meanwhile, shows the heat shield 132 230 when all the movable elements 132A, 132B, 132C, 132D, 132E are nested within each other. The moving elements 132A, 132B, 132C, 132D, 132E are here formed of cylinders made of the same material, for example a metallic material, such as steel or aluminum.
    [0017] As a variant, the movable elements may consist, for example, of quartz, glass or silica cylinders, whose external face facing the electrical resistors is coated with a layer reflecting the thermal radiation emitted by these electrical resistors, for example a metal layer, such as a layer of silver, aluminum, or gold.
    [0018] The evaporation means also comprise actuating means for sliding the movable elements 132A, 132B, 132C, 132D, 132E relative to one another to adjust the height of the heat shield 132. Although in the figures 2 to 12 the movable elements 132A, 132B, 132C, 132D, 132E are five in number and all have the same height, it can be envisaged alternatively that the evaporation means comprise more or less moving elements and that these they have different heights. This may especially be advantageous in order to adapt the height of the heat shield to the height of the evaporation chamber and to adjust this height with more or less precision. Finally, the evaporation means comprise the cylindrical body 101 of the evaporation chamber 100 which comprises a transparent wall which is chosen so as to transmit the infra-red radiation emitted by the electrical resistors 131. Under the pressure conditions prevailing at inside the outer enclosure 11, the heat exchanges between the electrical resistances 131 and the body 111, 121 of a crucible 110, 120 engaged with the evaporation chamber 100 are essentially by radiation, because the exchanges by The transparent wall may for example be formed of a hollow cylinder made of quartz, glass or silica, optionally coated with a layer improving the infra-red transmission. of the transparent wall.
    [0019] The heat shield 132, arranged between the electrical resistances 131 and this transparent wall of the body 101 of the evaporation chamber 100, will thus act as a mirror for the infra-red light radiated by the electrical resistances 131 towards the body 111 , 121 of a crucible 110, 120 being in the evaporation chamber 100.
    [0020] Thus, thanks to the heat shield 132, it is possible to discover all or part of the electrical resistances 131, so that only the fraction of material 7 contained in the upper part 114, 124 of the crucibles 110, 120, is subjected to radiation emitted by the electrical resistances and is heated, depending on the pressure in the evaporation chamber, to a heating temperature sufficient to allow its evaporation. Moreover, thanks to the actuating means sliding the movable elements 132A, 1328, 132C, 132D, 132E, it is possible to finely adjust the height of the heat shield 132 to adjust the flow of steam in real time 116, 126 (see Figures 4 and 8) through the necks 113, 123 of the crucibles 110, 120.
    [0021] In particular, it is possible to obtain evaporation conditions in which the vapor flow 116, 126 remains substantially constant throughout the evaporation of the material 7 contained in the crucibles 110, 120. This is particularly interesting for depositing a uniform layer on the substrate 2 placed in the vacuum deposition chamber 20. The steam flow 116, 126 of the material 7 generated by the evaporation means 131, 132, 101 heating the crucibles 110, 120 located in the evaporation chamber 100 then passes through the outlet orifice 103 of the evaporation chamber 100 and is then transported to the injector 13 along the injection duct 14 of the cell. evaporation 10, injector 13 which, as seen previously, generates the upstream vapor flow 4 towards the substrate 2 placed in the vacuum deposition chamber 20.
    [0022] As represented in FIGS. 2 to 12, the evaporation cell 10 also comprises a loading chamber 200 adjacent to the evaporation chamber 100 and situated here below the external enclosure 11 of the evaporation cell 10. This loading chamber 200 is delimited by a containment chamber 202 and includes an access hatch 201 allowing: in the open position, to put the internal volume 209 of the loading chamber 200 in communication with the outside of the cell 10, for example with the room in which the vacuum deposition apparatus 1 is stored, and in the closed position, to isolate the internal volume 209 of the charging chamber 200 from the outside of the cell. evaporation 10.
    [0023] Advantageously, it is possible to add to the loading chamber, upstream thereof, an airlock placed in a neutral atmosphere, for example with an inert gas at a pressure close to the atmosphere. This airlock then makes it possible to fill crucibles intended to be introduced into the loading chamber with materials that oxidize in the open air, such as organic materials for example.
    [0024] As for the external enclosure 11 of the evaporation cell 10, there are provided, on the internal faces of the confinement enclosure 202, heating elements, for example heating resistors 206, intended to heat substantially homogenously the heating element. internal volume 209 of the loading chamber, and in particular the various elements that may be there as the crucibles 110, 120. The confinement chamber 202 of the loading chamber 200 comprises on its upper wall an opening located in view of the insertion opening 12 carrying the evaporation chamber 100, so that the charging chamber 200 is in communication with the evaporation chamber 100 through this insertion opening 12 when it does not is not blocked. The loading chamber 200 furthermore includes an additional pump 222 connected to the confinement enclosure 202 via a pumping conduit 221 for evacuating said charging chamber 200, for example when the latter has been returned to the air by the opening of the access hatch 201. In the loading chamber 200, there is further provided means for loading and unloading the crucibles 110, 120, here a carousel system and piston. More specifically, the loading chamber 200 first comprises a piston 212A at the upper end of which is fixed a plate 212 intended to accommodate the first crucible 110 or the second crucible 120. The piston 212A is movable in vertical translation, from so that the plate 212 can rise and fall along the axis of the piston 212A, between: - a "low" position (case of Figures 2, 6, and 7) in which the plate 212 is close to the bottom wall of the confinement chamber 202, and a "high" position (in the case of FIGS. 3, 4, 5, 8, 10, 11, and 12) in which the plate 212 is located at the insertion opening 12 of the evaporation cell 10. The low position allows the loading or unloading of the tray 212 with a crucible 110, 120.
    [0025] Once the crucible 110, 120 in place on the plate 212, it can mount vertically through the piston 212A and thus engage the crucible 110, 120 with the evaporation chamber 100 passing through the insertion opening 12 of the evaporation cell 10. The loading chamber 200 also comprises a carousel 211 mounted on an axis of rotation 211A for rotating the carousel 211. This carousel 211 is intended to receive the crucibles 110, 120 for their loading and unloading the tray 212. The carousel system 211 and tray 212 is particularly advantageous because it offers a small footprint for a given number of crucibles. Thus, the loading chamber size 200 and the pumping capacity of the additional pump 222 connected to the charging chamber 200 can be limited.
    [0026] As shown in FIG. 2B, thermal shielding means are provided which are interposed between the external enclosure 11 of the evaporation cell 10 and the charging chamber 200. More specifically, these thermal shielding means here comprise a connecting flange 17 for attaching the bottom wall 11C of the outer enclosure 11 to the upper wall of the charging chamber 200. This connection flange 17 has a connection opening 17A coaxial with the insertion opening 12 and comprises a network of coils 17B traversed by a cooling liquid (water, nitrogen, etc.). This connection flange 17 makes it possible in particular to thermally isolate the evaporation chamber 100 from the charging chamber 200 and to prevent the heat released by the various heating means 16 of the evaporation cell disruptive effect on a crucible 110, 120 placed in the charging chamber 200, and vice versa so as not to disturb the thermal gradient in the crucible 110, 120 during evaporation. In this way, it is possible to remove "hot" the first crucible 110 of the evaporation chamber 100 when it is hot, without waiting for its cooling. The second crucible 120 can thus be introduced into the evaporation chamber 100 as soon as the first crucible 110 is withdrawn, and the evaporation can resume as soon as the second crucible 120 is put to temperature. Moreover, thanks to the thermal shielding means 17 it is possible to charge the second crucible 120 in the charging chamber 200 while the evaporation of the first crucible 110 is in progress, despite the heat released by the evaporation means 131, 132 which heat the first crucible 110 This released heat has no significant thermal and detrimental effect on the second crucible 120 in the charging chamber 200. In particular, the temperature of the material 7 to be evaporated present in the crucible 120 remains below the evaporation temperature of the material. 7. To implement the reloading method according to the invention, it is finally provided means for closing the insertion opening 12 of the cell. evaporation 10 which, advantageously, are implemented during the engagement of a crucible 110, 120 with the evaporation chamber.
    [0027] In the exemplary embodiments shown in FIGS. 2 to 8 and 10 to 12, these closure means comprise a ring gasket 117, 127 fixed along the side wall 111, 121 of crucibles 110, 120, in the lower part of this, close to the bottom 115, 125 of the crucible 110, 120. The outer diameter of the seal 117, 127 is chosen so that, when a crucible 110, 120 is inserted into the evaporation chamber 100 through the piston 212A and to the tray 212 of the loading chamber 200, the seal 117, 127 comes into contact with the body 101 of the evaporation chamber 100.
    [0028] In this way, when a crucible 110, 120 is loaded inside the evaporation chamber 100, the seal 117, 127 makes it possible to seal the evaporation chamber 100 with respect to the chamber 200. In other words, thanks to the seal 117, 127 provided on the crucibles 110, 120, it is possible when engaging a crucible 110, 120 with the evaporation chamber 100, to isolate the loading chamber 200 vis-à-vis the evaporation chamber 100. In another embodiment shown in Figures 9A and 9B, the closure means comprise a seal 212B attached to the peripheral edge of the tray 212. From the same manner as before, the outer diameter of the seal 212B is chosen so that when a crucible (the first crucible 110 in the case of Figures 9A and 9B) is inserted into the evaporation chamber 100 through the piston 212A and the tray 212 of the loading chamber 200, the seal 212B comes into contact with a with the body 101 of the evaporation chamber 100 so as to seal the insertion opening 12 of the evaporation cell 10.
    [0029] As shown in FIG. 10, it is also possible to provide a valve 17 placed on the injection duct 14 of the evaporation cell 10. Advantageously, this valve 17 can be, for example, an "all-or-nothing" sealed valve. With two open and closed positions which allows in the closed position, when the evaporation chamber 100 is empty, to prevent the flow of vapor back to the evaporation chamber 100 and go towards the loading chamber 200 cooler to condense on the inner walls of the charging chamber 202. Alternatively, one could provide two valves placed in series on the injection duct: a first "all-or-nothing" type watertight valve and a second control valve downstream of the first sealed valve.
    [0030] Although the flow rate of the vapor stream at the outlet of the evaporation chamber is adjusted by means of evaporation, this control valve can also make it possible to regulate the flow of material vapor 7 even more finely. Preferably, these valves are placed in the outer enclosure 11 of the evaporation cell 10 so as to be heated during use to avoid condensation problems in these valves. Referring now to FIGS. 2 to 8, an exemplary implementation of the method for recharging the evaporation cell 10 of the vacuum deposition apparatus 1 will be described. It will be understood in the light of the description which will follow the advantages of such a reloading process in order to reduce the downtime of the vacuum deposition apparatus 1.
    [0031] It will be considered here, as shown in FIG. 2A, that the vacuum deposition apparatus 1 is in operation and that: a first crucible 110 is engaged with the evaporation chamber 100 of the evaporation cell 10 and heated by the evaporation means 131, 132 so as to generate a vapor flow 116 through the outlet orifice 103 of the evaporation chamber 100, and a previous crucible 130, whose contents have already been evaporated, is found inside the charging chamber 200. At this time, as explained above, the vacuum deposition chamber 20, the outer enclosure 11 which is in direct communication with the vacuum deposition chamber 20, and the chamber 100 are at a substantially identical pressure, close to a vacuum level, between 10-3 and 10-8 Torr. The first crucible 110, which is engaged in the evaporation chamber 100 of the evaporation cell 10, makes it possible, thanks to its seal 117, to isolate the loading chamber 200 from the adjoining evaporation chamber 100. and the vacuum deposition chamber 20. It is therefore possible to vent the loading chamber 200 without impacting the vacuum of the vacuum deposition chamber 20. Also, in a process loading step, it opens the access hatch 201 of the loading chamber 200 to remove the crucible 130 previously emptied. The pressure in the loading chamber 200 is then substantially greater than that prevailing in the vacuum deposition chamber 20, typically close to 1 atmosphere. From outside the evaporation cell 10 is then introduced, possibly from an airlock, generally called a "glove box", under a neutral atmosphere, the second crucible 120 inside the charging chamber 200 through the access trap 201, and this second crucible 120 is deposited on the carousel 211 of the charging chamber 200. After the step of introducing the second crucible 120 into the charging chamber 200, a step of confinement of the it. This confinement step is intended to reduce the pressure inside the charging chamber 200 to a level comparable to that of the evaporation chamber 100 during the evaporation of the first crucible 110, namely approximately 10-3 to 10. -8 Torr. During this confinement step, the access hatch 201 of the loading chamber 200 is closed in leaktight manner with respect to the outside of the evaporation cell 10, and thanks to the additional pump 222, pumping is carried out inside the charging chamber 200 so as to reach the aforesaid pressure level. The pressure levels in the charging chamber 200 and in the evaporation chamber 100 are then comparable, so that the plate 212 supporting the first crucible 110 can be removed without significant effort and without risk of breakage. During the loading and confinement steps, it is understood that the flow of vapor 116 generated by the first crucible 110 heated by the electrical resistors 131 and the heat shield 132 does not stop and therefore that the level of the material 7 in the first crucible 110 decreases (case of Figures 3 and 4) until the first crucible 110 is empty (case of Figure 5) or until the level of material 7 in the first crucible 110 is less than a predetermined minimum threshold. It is then possible to release the first crucible 110 from the evaporation chamber 100 by actuating the piston 212A downwards, which allows the first crucible 110 to be transferred from the evaporation chamber 100 to the loading chamber 200. In other words, during the release step, the first crucible 110 is removed from the evaporation chamber 100 by passing it through the insertion opening 12 of the evaporation cell 10 which communicates the charging chamber 200 and the evaporation chamber 100.
    [0032] It is then in the situation shown in Figure 6 where the first crucible 110, empty, rests on the plate 212 in the low position, and where the second crucible 120, full, is on the carousel 211 loading. By rotation of the carousel 211 (see Figure 7), it is then possible to interchange the first crucible 110 with the second crucible 120, so that it is positioned on the plate 212 of the charging chamber 200. The second crucible 120 can then be engaged with the evaporation chamber 100 by actuating the piston 212A upwards. The second crucible 120 is thus inserted into the evaporation chamber 100 through the insertion opening 12 (see FIG. 8).
    [0033] It should be noted here that, thanks to the seal 127 attached to the body 121 of the second crucible 120, the engagement step of the second crucible makes it possible to seal the insertion opening 12 in a sealed manner so that the engagement step causes the loading chamber 200 to be isolated from the evaporation chamber 100 of the evaporation cell, and also from the vacuum deposition chamber 20 of the vacuum deposition apparatus 1.
    [0034] As previously explained for the first crucible 110, once the isolation ensured by the engagement of the second crucible 120, it is then possible to discharge the first crucible 110 from the charging chamber 200, for example to introduce one or more new crucibles when charged with the evaporation chamber 100 (see FIG. 8), the second crucible 120 can be put into evaporation conditions by means of evaporation means for generating a flow of steam 126 of the material through the outlet orifice of the evaporation chamber 100. It is thus clear that the reloading method according to the invention makes it possible to reduce the duration during which the flow of material vapor is interrupted. . Indeed, this interruption is limited in time by the operations of releasing the first crucible 110 and engaging and setting evaporation conditions of the second crucible 120. The crucibles 110, 120 being of small volume, their setting in conditions Evaporation can be rapid because the amount of material 7 to be heated is limited.
    [0035] In this sense, it can be considered that the reloading process of the evaporation cell 10 according to the invention allows the vacuum deposition apparatus 1 to operate in a quasi-continuous production regime. Advantageously, it is also possible, before the engagement of the second crucible 120 with the evaporation chamber 100, to prepare the second crucible 120 then placed in the charging chamber 200 in order to further reduce the interruption time of the steam flow. This preparation step is intended to reduce the duration of the step of setting evaporation conditions of the second crucible 120.
    [0036] More particularly here, the heating means 206 of the charging chamber 200 are used to preheat the second crucible 120 to a predetermined preheating temperature. Preferably, the power of the heating means is adjusted so that the preheating temperature is lower than the evaporation temperature of the material 7 contained in the second crucible 120 so as to prevent the beginning of the evaporation of said material 7. Although the reloading method according to the invention has been described with only one crucible waiting in the charging chamber, it can easily be implemented with several crucibles.
    [0037] For example, during the reloading stage, it is possible to introduce as many crucibles as the carousel can accommodate. In this case, the opening of the access door of the loading chamber and the use of the additional pump are less frequent and the conditions of temperature and pressure in the loading chamber are more stable. Each time an empty crucible is changed, one of the solid crucibles remaining on the carousel is inserted. When all the crucibles present on the carousel are empty (a crucible being evaporating in the evaporation chamber) Furthermore, as shown in FIG. 12, the recharging process according to the invention can be used to a vacuum deposition apparatus 1 with an evaporation cell 10 comprising two evaporation chambers 100, 300.
    [0038] It will be understood from the following description that a continuous production of material vapor by the evaporation cell is possible. In the example described here, these two evaporation chambers 100, 300 are identical to the evaporation chamber 100 previously described (see FIGS. 2 to 11) and the respective evaporation means 131, 132, 311, 312 are also identical. The evaporation chambers 100, 300 are connected in parallel to the injection duct 14 respectively by means of duct portions 141, 142 connected to the outlet orifices 103, 303 of said evaporation chambers 100, 300.
    [0039] Between the two evaporation chambers 100, 300 are disposed in the evaporation cell 10, heat shields of refractory material such as aluminum in order to thermally independent these two evaporation chambers 100, 300. The outer enclosure 11 of the evaporation cell 10 has two insertion openings 12, 12B for the engagement and disengagement of the crucibles. In correspondence, the containment enclosure 202 of the loading chamber 200 comprises on its upper wall two openings located opposite these insertion openings 12, 12B, so that the loading chamber 200 is respectively in communication with the first evaporation chamber 100 and the second loading chamber 300 through the first insertion opening 12 and the second insertion opening 12B, when these are not closed. Furthermore, the loading chamber 200 comprises, in addition to the carousel 211 and the first plate 212, a second plate 213 associated with its piston 213A, which allows the release and insertion of a crucible in the second evaporation chamber 300. The carousel 211 is arranged in the loading chamber 200 so as to deposit a crucible on one or other of the trays 212, 213. We will now describe the reloading process according to the invention and see how the it allows continuous production. It is considered here that the initial situation of the evaporation cell is that represented in FIG. 12: a first crucible 110, almost empty, placed in the first evaporation chamber 100, is being evaporated and generates a flow of vapor 116 of material 7 through the outlet orifice 103, vapor flow 116 then leads to the injector 13 (not shown) through the portion 141 of conduit and the injection conduit 14; a second crucible 120, solid, placed in the charging chamber 200 evacuated by the additional pump 222, is waiting on the carousel 211 and preheated by the heating means 206 of the charging chamber 200; a third crucible 330, solid, engaged with the second evaporation chamber 300, is progressively brought into evaporation conditions thanks to the electric resistors 311 heating the third crucible 330 through the heat shield 312 and the body 301 of the chamber Advantageously, it is provided that the third crucible 330 engaged with the second evaporation chamber 300 begins its evaporation when the quantity of material 7 to be evaporated remaining in the first crucible 110 is below a predetermined minimum threshold. , so as to maintain a constant flow rate for the material flow conducted in the injection conduit 14 to the injector 13. It is also possible to install "all-or-nothing" type watertight valves and / or valves of regulation on the portions 141, 142 of the injection duct 13, either to regulate the flow of vapor inside the injection duct, or to prevent the flu x of steam leaving one of the evaporation chambers pollutes the other evaporation chamber. When the first crucible 110 is empty or when the quantity of material 7 to be evaporated remaining in the first crucible 110 is less than a predetermined low limit (this lower limit being less than the previous minimum threshold), its replacement is carried out by reloading the Evaporation cell 10. At this time, the second evaporation chamber 300 takes over, the vapor flow generated by the third crucible 330 being directed towards the injector 13, so that the flow of steam injected into the vacuum deposition chamber 20 is not interrupted.
    [0040] During this reloading, the first crucible 110 is released from the first evaporation chamber 100 by passing it through the first insertion opening 12 thanks to the plate 212. Then, the first crucible 110 is discharged from the plate 212 onto the carousel 211 and the second crucible 120 of the carousel 211 is loaded onto the plate 212.
    [0041] The second crucible 120 is then engaged with the first evaporation chamber 100 and is gradually brought into evaporation conditions so that, when the quantity of material 7 to evaporate remaining in the third crucible 110, which is being evaporated. in the second evaporation chamber 300, is below the predetermined minimum threshold. Once the second crucible 120 engaged with the first evaporation chamber 100, the charging chamber 200 is isolated from the two evaporation chambers 100, 300, and also the vacuum deposition chamber 20. It is then time to open the access hatch 201 of the loading chamber 200 to remove the first crucible 110 and introduce a fourth crucible (not shown) into the loading chamber 200 to the air, the pressure in the loading chamber 200 being then substantially greater than that prevailing in the vacuum deposition chamber 20. Finally, one can proceed to the confinement step of the charging chamber 200 to reduce the pressure inside this charging chamber 200 to a level comparable to that of the evaporation chambers 100, 300. When the third crucible 330 is to be emptied, it is possible to implement, according to the recharging method according to the invention, the steps of releasing the third crus 330, and engaging and evaporation of the fourth crucible engaged with the second evaporation chamber 300. Thus, by putting the recharging process according to the invention with an evaporation cell having at least two evaporation chambers and a loading chamber adjoining said evaporation chambers, it is possible to never interrupt the flow of material vapor transported to the injector to be injected into the vacuum deposition chamber of the apparatus vacuum deposition. It is therefore possible to provide a continuous production, with a scroll of substrates facing said injector.
    [0042] In order to limit the frequency of recharging of the evaporation cell, it is advantageous to provide in the external enclosure of the evaporation cell a cylinder having a large number of evaporation chambers, each provided with their own means of evaporation. evaporation and possibly their own valve system at the outlet of said chambers. This barrel can be loaded at one time by means of a "charger" bringing together a number of crucibles corresponding to the number of evaporation chambers, the installation of the charger to simultaneously engage all the crucibles in their room d respective evaporation.
    [0043] The method of reloading the evaporation cell then comprises: a step of loading a second charger unit, bringing together a plurality of crucibles each containing the material to be evaporated, in a previously isolated charging chamber of said adjacent evaporation chambers; barrel, the pressure in said loading chamber then being substantially greater than that prevailing in the vacuum deposition chamber, - after said introduction step, a step of confining said loading chamber intended to reduce the pressure to the inside said loading chamber at a level comparable to that of the evaporation chambers of the barrel, after said confinement step, a step of releasing said first magazine from said barrel during which said first magazine transferred from said barrel to said barrel loading chamber, - after said step of releasing the first loader, a step of engagement of said second charger with said barrel of evaporation chambers, and - after said step of engaging said second crucible, a step of setting evaporation conditions of said crucibles of the second charger.
    权利要求:
    Claims (7)
    [0001]
    REVENDICATIONS1. Method for reloading an evaporation cell (10) for evaporating a material (7) for deposition on a substrate (2) placed in a vacuum deposition chamber (20), a first crucible (110) containing said evaporating material (7) being engaged with an evaporation chamber (100) of said evaporation cell (10), evaporation means (101, 131, 132) being provided for placing said first crucible (110) ) under evaporation conditions for generating a vapor stream (116) of the material (7) through an outlet (103) of said evaporation chamber (100), said outlet port (103) being connected an injector (13) for injecting said vapor into said vacuum deposition chamber (20), said charging method comprising: - a step of loading a second crucible (120) containing the material (7) to evaporating in a charging chamber (200) previously isolated from said evaporation chamber (1 00), the pressure in said loading chamber (200) being then substantially greater than that prevailing in the vacuum deposition chamber (20), - after said introducing step, a step of confining said loading chamber ( 200) for reducing the pressure inside said charging chamber (200) to a level comparable to that of said evaporation chamber (100) upon evaporation of said first crucible (110), - after said step confinement, a step of releasing said first crucible (110) from said evaporation chamber (100) during which said first crucible (110) is transferred from said evaporation chamber (100) to said loading chamber ( 200), after said step of releasing the first crucible (110), a step of engaging said second crucible (120) with said evaporation chamber (100), and - after said step of engaging said second crucible (120) , a step of m ise under evaporation conditions of said second crucible (120) for generating a vapor stream (126) of the material (7) through said outlet port (103) of the evaporation chamber (100).
    [0002]
    2. The method of reloading according to claim 1, wherein during said step of engaging said second crucible (120), said charging chamber (200) is isolated from said evaporation chamber (100) and of said vacuum deposition chamber (20).
    [0003]
    3. reloading method according to one of claims 1 and 2, wherein in said step of loading said second crucible (120), is opened an access door (201) of said loading chamber (200) and introduced from outside said evaporation cell (10), said second crucible (120) into said loading chamber (200) through said access door (201).
    [0004]
    4. A reloading method according to claim 3, wherein during said confinement step, said access hatch (201) is closed in leaktight manner with respect to the exterior of said evaporation cell (10). and pumping is performed within said charging chamber (200).
    [0005]
    5. Reloading method according to one of claims 1 to 4, wherein: during said step of releasing the first crucible (110), said first crucible (110) is removed from said evaporation chamber (100) in passing it through an insertion opening (12) communicating said charging chamber (200) and said evaporation chamber (100), and - during said step of engaging said second crucible (120) inserting said second crucible (120) into said evaporation chamber (100) by passing it through said insertion opening (12) and sealing said insertion opening (12) to isolate said loading chamber (200) of said evaporation chamber (100).
    [0006]
    6. A method of recharging according to one of claims 1 to 5, comprising, before said step of engaging said second crucible (120) with said evaporation chamber (100), a step of preparing said second crucible (120) in said charging chamber (200) for reducing the duration of said evaporation step of said second crucible (120).
    [0007]
    7. The method of reloading according to claim 6, wherein said preparation step comprises a step of preheating said second crucible (120) in said charging chamber (200) to a predetermined preheating temperature.
    类似技术:
    公开号 | 公开日 | 专利标题
    EP2915897A1|2015-09-09|Method for refilling an evaporation cell
    EP0334432B1|1993-10-13|Epitaxy reactor with wall protected against deposits
    FR2878863A1|2006-06-09|VACUUM DEPOSITION DEVICE WITH RECHARGEABLE RESERVOIR AND CORRESPONDING VACUUM DEPOSITION METHOD.
    KR101363147B1|2014-02-13|Deposition method and deposition apparatus
    EP2271790B1|2016-06-15|Device and process for chemical vapor phase treatment
    US6275649B1|2001-08-14|Evaporation apparatus
    EP1466031B1|2010-11-17|Method and installation for the densification of substrates by means of chemical vapour infiltration
    EP0249516B1|1990-07-25|Cell for epitaxial growth by molecular jets, and associated process
    FR2956411A1|2011-08-19|SYSTEM FOR HEATING A VAPOR PHASE DEPOSITION SOURCE
    EP2937443A1|2015-10-28|Evaporation cell
    EP1307606B1|2006-03-08|Barrier coating
    CH650275A5|1985-07-15|APPARATUS FOR PERFORMING THE REACTIVE DEPOSITION OF AN OXIDE COATING ON A SUBSTRATE.
    EP2769001B1|2017-12-20|Injection system for an apparatus for depositing thin layers by vacuum evaporation
    EP1458902A1|2004-09-22|Method and installation for densifying porous substrate by gas-phase chemical infiltration
    EP2682503B1|2016-12-14|Evaporation device for a vacuum-deposition apparatus and vacuum-deposition apparatus including such an evaporation device
    EP2025773A1|2009-02-18|Vacuum evaporation apparatus for solid materials
    EP0236639B1|1990-03-14|Flexible automatic installation for performing a fast thermochemical treatment
    US20090020070A1|2009-01-22|Vacuum evaporation apparatus for solid materials
    US6473564B1|2002-10-29|Method of manufacturing thin organic film
    KR101286803B1|2013-07-17|Organic compound steam generator and apparatus for producing organic thin film
    FR2909990A1|2008-06-20|METHOD AND APPARATUS FOR THE MANUFACTURE OF BLOCKS OF A SEMICONDUCTOR MATERIAL
    FR2824663A1|2002-11-15|Silicon plate doping, diffusion or oxidation procedure and apparatus comprises oven subjected to constant depression as gas is introduced
    FR2956412A1|2011-08-19|CONSTANT VOLUME SHUT-OFF VALVE OF A VAPOR PHASE DEPOSITION SOURCE
    EP2593242B1|2017-11-15|Method for depositing a layer on the surface of a substrate
    EP3464207A1|2019-04-10|Process for forming a barrier coating at the surface of a container and related facility
    同族专利:
    公开号 | 公开日
    KR20150103641A|2015-09-11|
    CN104911545A|2015-09-16|
    JP2015166492A|2015-09-24|
    FR3018082B1|2016-03-18|
    US20150247234A1|2015-09-03|
    EP2915897A1|2015-09-09|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US20050034671A1|2003-08-15|2005-02-17|Semiconductor Energy Laboratory Co., Ltd.|Deposition apparatus and manufacturing apparatus|
    JP2005179764A|2003-12-24|2005-07-07|Hitachi Zosen Corp|Vapor deposition apparatus|
    WO2006001205A1|2004-06-28|2006-01-05|Hitachi Zosen Corporation|Evaporator, vapor deposition apparatus, and method of switching evaporator in vapor deposition apparatus|
    CN106637383A|2016-11-17|2017-05-10|珠海鼎泰芯源晶体有限公司|Crystal growing furnace capable of realizing continuous production|
    CN107893212B|2017-12-18|2019-12-20|信利（惠州）智能显示有限公司|Continuous evaporation equipment|
    CN107955969A|2017-12-28|2018-04-24|河北同光晶体有限公司|A kind of SiC single crystal growing system being persistently fed|
    DE102019104988A1|2019-02-27|2020-08-27|VON ARDENNE Asset GmbH & Co. KG|Supply device, method and processing arrangement|
    CN112301427A|2020-11-18|2021-02-02|阳光能源（青海）有限公司|Graphite heating device for monocrystalline silicon production and heating method thereof|
    法律状态:
    2015-12-03| PLFP| Fee payment|Year of fee payment: 3 |
    2016-12-01| PLFP| Fee payment|Year of fee payment: 4 |
    2017-12-01| PLFP| Fee payment|Year of fee payment: 5 |
    2019-12-02| PLFP| Fee payment|Year of fee payment: 7 |
    2020-12-02| PLFP| Fee payment|Year of fee payment: 8 |
    2021-12-01| PLFP| Fee payment|Year of fee payment: 9 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1451712A|FR3018082B1|2014-03-03|2014-03-03|METHOD FOR RECHARGING EVAPORATION CELL|FR1451712A| FR3018082B1|2014-03-03|2014-03-03|METHOD FOR RECHARGING EVAPORATION CELL|
    EP15305308.7A| EP2915897A1|2014-03-03|2015-02-27|Method for refilling an evaporation cell|
    US14/635,296| US20150247234A1|2014-03-03|2015-03-02|Method for reloading an evaporation cell|
    JP2015040905A| JP2015166492A|2014-03-03|2015-03-03|Method of re-loading evaporation cell|
    CN201510164034.9A| CN104911545A|2014-03-03|2015-03-03|Method for reloading an evaporation cell|
    KR1020150029787A| KR20150103641A|2014-03-03|2015-03-03|Method for reloading an evaporation cell|
    [返回顶部]