DE102009009022A1 - Method and device for coating flat substrates with chalcogens - Google Patents

Abstract

The invention relates to a method and a device for coating flat substrates with chalcogens in the form of thin layers. With the invention, a rapid and cost-effective coating of sheet-like substrates with chalcogens, with a controlled and safe removal of the non-condensed chalcogen and a device suitable for carrying out the method should be made possible. This is achieved by forming an inlet and outlet gas lock (6, 7) for oxygen-tight closure of a process chamber (5), introducing one or more substrates to be coated and tempered to a predetermined temperature into the process chamber (5), introducing a chalcogen vapor / Carrier gas mixture in the process chamber (5) having a transport channel (4) above the substrates, forming a flow of the chalcogen vapor / carrier mixture through the transport channel (4) between the input and output gas locks (6, 7) and forming a chalcogen layer on the substrates by means of PVD for a given residence time and removal of the non-condensed on the substrates chalcogen vapor and the carrier gas between the gas locks, and removal of the substrates after the predetermined process time.

Description

The The invention relates to a method and a device for coating of flat substrates with chalcogens, in the form of thin ones Layers in a process chamber.

chalcogen for example, in a multi-stage process for the production of thin film modules based on Compound semiconductors needed. Chalcogens include the elements Sulfur, selenium, tellurium and polonium. Oxygen belongs Although also to the chalcogens, but is in the production of Thin-film modules undesirable.

at this process is applied in a first step to the substrate, which, for example, a glass substrate with a molybdenum layer may be, metallic precursor layers and a chalcogen layer applied. The metallic precursor layers can Contain copper (Cu), gallium (Ga) and indium (In) and can applied to the substrate by known technologies, such as sputtering become. The subject of the present invention is a method and a device for applying a chalcogen layer, preferably one Selenium layer with the aim of converting the layer stack into one semiconducting layer.

This is done in a second step. This is achieved with a post-published procedure ( PCT / EP 2008/007466 ), in which the prepared substrates in an oven segmented in several temperature ranges at a pressure at about atmospheric pressure in several steps each heated to a predetermined temperature up to the final temperature between 400 ° C and 600 ° C and while maintaining the final temperature in semiconducting layers being transformed.

To The prior art also includes methods for the coating became known with chalcogens, which proceed in a vacuum. there Chalcogens are thermally evaporated in vacuo and on the substrates deposited.

vacuum is usually used to coat with chalcogens Among other things, to exclude the access of oxygen. In the presence of oxygen, for example, selenium would to react to a toxic compound (selenium dioxide) that is responsible for the other processes, such as thermal conversion the precursor layers in semiconducting layers, disturbing would.

vacuum processes usually result in industrial mass production at high cost. Pumping and lock times lead to increased Cycle times and thus always too low in addition to long process times Productivity.

A process for the vapor deposition of the vapor phase under a protective gas on a flexible substrate, wherein simultaneously or sequentially sodium and / or sulfur are deposited by condensation on the continuous band, has been described in US Pat DE 10 2004 024 601 disclosed. The device for the separation consists of a reactor with source zone, transport zone and condensation zone, wherein an inert trailing gas dilutes the selenium, sulfur and sodium vapor and transported from the different temperature controlled sources for condensation on the precursor. In this case, the precursor is temperature-controlled to less than 100 ° C, so that only a condensation, but not a reaction of the components of the precursor with the selenium, sodium and / or sulfur vapor takes place.

A rapid and cost-effective coating process for chalcogens, in particular for applying thin layers of the chalcogens in the range of 100 nm to 10 μm on large-area substrates, as well as a device suitable for carrying out the process has been described in the patent application no. PCT / EP 2008/062061 created.

The Method is realized by forming an input and output side Gas curtain for the oxygen-tight closure of a transport channel in a Aufdampfkopf, introducing an inert gas into the transport channel for the displacement of atmospheric oxygen, Introducing one or more to be coated and to a given one Temperature-tempered substrates in the transport channel of the process chamber, Introducing a chalcogen vapor / carrier gas mixture a source in the transport channel of the vapor deposition over the substrates and forming a chalcogen layer on the substrates by means of physical vapor deposition (PVD) under a predetermined Pressure, as well as removal of the substrates after expiration of the given Process time.

at only a part of the chalcogen vapor condenses in the process mentioned on the substrates. The rest of the chalcogen vapor must therefore be controlled be removed.

Of the Invention is now the object of a method and a Apparatus for coating flat substrates with chalcogens in the form of thin layers, in particular of sheetlike Substrates prepared with precursor layers from any desired Materials, preferably of glass substrates, in a controlled Declare the discharge of the uncondensed chalcogen.

The The object underlying the invention is achieved by a method solved by forming an input and output side Gas lock for the oxygen-tight closure of a process chamber, Introducing one or more to be coated and to a given one Temperature tempered substrates in a transport direction in the process chamber, initiating one across the width of the Substrates evenly distributed chalcogen vapor / carrier gas mixture in the transport channel having a process chamber above the Substrates, forming a flow of the chalcogen vapor / carrier gas mixture over the substrates through the transport channel between the input and output side gas locks, forming a chalcogen layer on the substrates by means of PVD during a given time Residence time and removal of the excess not condensed on the substrates Chalcogen vapor and the carrier gas between the gas locks, and removal of the substrates from the process chamber after a specified process time.

For the gas locks and / or as carrier gas can be an inert gas, preferably nitrogen can be used.

In In one embodiment of the invention, the chalcogen vapor / carrier gas mixture flows, after introduction into the process chamber above the substrates along the transport chamber in or against the transport direction above the substrates along before the chalcogen vapor / carrier gas mixture is removed again.

Farther the substrates are preferred during the coating Moved in the transport direction, with the movement at a constant speed can be done.

It is further advantageous if the substrates prior to introduction tempered in the process chamber to a temperature below 200 ° C. be, for. B. to a temperature between 20 ° C and 100 ° C. or also room temperature.

Farther can the substrates during the coating to a temperature below 200 ° C, preferably between 20 ° C and 100 ° C, tempered.

The The object underlying the invention is further in a device for coating flat substrates with chalcogenes in the form of thin layers in a process chamber, with an opening for insertion and an opening for spreading the flat Substrate is provided, and an input-side gas lock on the opening for introducing the substrates and an output side Gas lock at the opening for discharging the substrates and with a means of transport for the flat Substrates is provided by the process chamber, solved by that in the transport opposite wall of the Process chamber between the gas locks an opening to Supply of a chalcogen vapor / carrier gas mixture and lateral offset to an opening for removal of the chalcogen vapor / carrier gas mixture are present.

The openings for insertion and removal and allow the gas locks it, the device in a continuous process, at a pressure in the Near atmospheric pressure and below defined Residual gas conditions, especially with the exclusion of oxygen, to operate.

The Means of transport and the openings for insertion and removal allow introduction of one or more substrates to be coated into the process chamber, transporting the substrates through the process chamber through and an application of the coated Substrates out of the process chamber.

The Coating takes place between the openings for feeding and removal of the chalcogen vapor / inert gas mixture instead of. The chalcogen vapor / carrier gas mixture is over the opening for supplying the chalcogen vapor / carrier gas mixture introduced into the process chamber. The suction over the another opening leads to a flow of the chalcogen vapor / carrier gas mixture along the process chamber. This is a particularly uniform coating achieved.

The Transport means preferably allows movement of the Substrates at a constant speed.

The Device can be operated so that the chalcogen vapor / carrier gas mixture flows in or against the transport direction.

is the transport direction of the substrates in the direction of the flow of chalcogen vapor / carrier gas mixture, the relative Rate of chalcogen vapor to the substrate opposite the flow rate of the chalcogen vapor / carrier gas mixture be reduced. This allows for improved deposition of the chalcogen on the substrates.

If, however, the device is operated such that the transport direction of the substrates is directed against the flow of the chalcogen vapor / carrier gas mixture along the process chamber, this can compensate for existing density fluctuations of the chalcogen vapor along the process chamber and to a more uniform coating to lead.

The Device is arranged so that the chalcogen vapor / carrier gas mixture mainly over an area of in the process chamber located substrates flows. It forms by PVD a chalcogen layer on itself in the process chamber located substrates.

Of the Chalcogen vapor which is not condensed on the substrates with the carrier gas together over the opening for removal from the process chamber and then over at least one exhaust pipe removed. The chalcogen can subsequently, for example with the help of a condensation trap and / or a filter. The accumulated waste of chalcogen must either be disposed of or sent for reprocessing become.

In a continuation of the invention is another laterally offset opening for feeding a Chalcogen vapor / carrier gas mixture in the transport opposite wall of the process chamber. The openings are for Supply and discharge offset in the transport direction to each other, in particular, the openings for the supply and discharge in the order of feeding, discharging and feeding arranged.

The Pressure conditions in the chamber are adjusted so that defined streams from the openings to the feeder of the chalcogen vapor / carrier gas mixture to the center of the process chamber be generated.

The Coating takes place between the openings for feeding of the chalcogen vapor / carrier gas mixture. Through this Arrangement, the area in which a coating takes place be easily doubled.

It It is understood that the number of openings to the supply and Removal of a chalcogen vapor / carrier gas mixture not limited to two or three.

To the better exclusion of, for example, oxygen in the process chamber the process chamber can be surrounded by a housing. The housing has two opposite openings and a transport channel in between for insertion and Application of the substrates by means of the transport, which is extends through the process chamber. The openings in the housing define a subspace of the space enclosed by the housing, the so-called transport channel.

This allows introduction of the substrates in the transport channel at an opening of the case, a transport the substrates through the transport channel and thus through the Process chamber through, and finally an application the substrates at the other opening of the housing.

Chalkogendampf which from the process chamber in the surrounded by the housing Room should be able to escape, for example, with the help of a separate Housing extraction can be removed.

The Housing can, for example, from a box made of Plexiglas consist. This allows optical monitoring the process chamber by the user.

The Input and output side gas locks of the process chamber can each consist of two gas curtains. It can also be one additional suction between the two gas curtains to be available.

This allows the gas flows on both sides of the To adjust the gas lock independently of each other.

When Protective / carrier gas is preferably an inert gas such as Example nitrogen used.

The Protective gas of the respective outer gas curtains For example, about the suction of the housing to the outside and the protective gas of each inner gas curtains over the opening for the extraction of the chalcogen vapor / carrier gas mixture in the process chamber inwards, into the process chamber, sucked become.

This ensures a separation of the atmosphere in the process chamber from the atmosphere outside the process chamber.

A Embodiment of the invention includes a device which it allows the substrates to a temperature below 200 ° C, for example, to a temperature between 20 ° C and 100 ° C, to temper.

The Tempering device can, for example, by a cooling device be realized because the substrates in the hot atmosphere be heated in the process chamber.

Farther can be used for components that come into contact with chalcogen vapor a heating device may be provided. Should chalcogen steam on condense these components, can by targeted heating, for example, during a maintenance, the chalcogen evaporate again and removed, for example, via the housing exhaust become.

In a continuation of the invention, the openings for the supply and discharge of the chalcogen are vapor / carrier gas mixture slit-shaped openings which are aligned perpendicular to the transport direction and which extend over the entire substrate located in the process chamber. This has the advantage of a more uniform coating.

Farther The wall of the process chamber can be placed over the substrates between the slot-shaped openings for supply and discharge be wavy. The wave crests are parallel to the slot-shaped openings, that is perpendicular to the transport direction along the transport channel, aligned.

to Feeding the chalcogen vapor / carrier gas mixture over the corresponding openings, for example, can be any opening for supplying the chalcogen vapor / carrier gas mixture with a vaporization chamber over one or more Ducts through which the chalcogen vapor / carrier gas mixture flows, be connected.

The Lines can run along a slot-shaped opening for supplying the chalcogen vapor / carrier gas mixture distributed end to an even distribution of the chalcogen vapor / carrier gas mixture over the to receive the entire opening.

In a further development of the invention, the lines which lead to a slot-shaped opening in the lower part of the lines the shape of the slot-shaped opening accept. This allows a nearly uniform Distribution of the chalcogen vapor / carrier gas mixture via the entire slot-shaped opening away.

Farther The lines in the lower part can be followed with constrictions be provided by relaxation zones.

This causes the chalcogen vapor / carrier gas mixture which flows through these constrictions dammed up and thus compressed and then expanded again. This process is repeated. Thereby the chalcogen vapor / carrier gas mixture is distributed the desired length and allows a homogeneous coating of the substrates.

For a uniform suction of the chalcogen vapor / carrier gas mixture over the entire slit-shaped opening for suction of the chalcogen vapor / carrier gas mixture the exhaust pipes to the slot-shaped opening take the form of the slot-shaped opening and be provided with constrictions followed by relaxation zones.

The Evaporation chamber is a chamber with at least one outlet to remove the chalcogen vapor / carrier gas mixture to which the cables connect. The chamber can at least one additional input to supply solid chalcogen and an access for the feeder have a carrier gas.

The solid chalcogen melts in the heatable evaporation chamber and forms a lake Selensee. For dossing the amount of chalcogen, the chamber be equipped with a level sensor.

The Carrier gas which enters the chamber and preferably previously heated, takes in the chamber chalcogen vapor and the chalcogen vapor / carrier gas mixture is over one or more conduits of an opening for delivery fed to the chalcogen vapor / carrier gas mixture.

Around the flow rate with the carrier gas to control the chamber flows, it can be monitored by a flow meter and over a fine regulating valve can be adjusted. It is understood that the control can run automatically.

Around a return flow from an opening to the feeder of the chalcogen vapor / carrier gas mixture to a vaporization chamber can prevent an additional carrier gas feed in each line between the evaporation chamber and the opening be provided for feeding. The so-called process additive gas, which is introduced by these additional feeds while creating a suction that the chalcogen vapor / carrier gas mixture sucked out of the chamber.

Around the flow rate at which the process additive gas in a line between the evaporation chamber and the opening for supplying the chalcogen vapor / carrier gas mixture flows, can control each line with a flow meter and adjusted via a fine regulating valve.

A increased flow rate of the process additive gas leads to a larger chalcogen vapor / carrier gas flow in the associated line between the evaporation chamber and slit-shaped opening for feeding of the chalcogen vapor / carrier gas mixture.

With the independent regulation of process additive gas flows can the homogeneity of the deposition perpendicular to the transport direction be further improved.

Since, as already described, not all the chalcogen vapor on the substrates never derschlägt, this chalcogen vapor / carrier gas mixture must be discharged as exhaust gas through the opening to the suction. To limit the loss of chalcogen, this offgas can be split by a flow divider. One part is then further discharged as exhaust gas, called residual exhaust gas, the other part can be made available to the coating again, for example via the additional carrier gas feeds or via the carrier gas feeds of the chambers. The temperature of the recirculated chalcogen vapor / carrier gas mixture should never fall below the condensation temperature of the chalcogen to avoid condensation of the chalcogen in the recirculation.

In a continuation of this exhaust gas recirculation Chalkogen is withdrawn from the residual exhaust gas and again the coating recycled gas enriched with chalcogen.

to Feeding the solid chalcogen into the evaporation chamber can at least one feeding device in the device to be built in. A feeding device may consist of a Container which can be funnel-shaped and which provides a supply of chalcogen, a metering device that it allows a given amount over at least one Piping into an evaporation chamber, and a valve exist for each pipeline. The valves are during open and stay open to the feed of the chalcogen otherwise closed, so that as far as possible an escape of chalcogen vapor from the evaporation chamber into the feed device is prevented in it.

at large systems for coating substrates with chalcogens can have multiple inputs to supply with solid chalcogen a uniform distribution be ensured in a chamber. In this case, a feed device solid chalcogen evenly on the different ones Distribute inputs to a chamber, or it can also be used for each input provided a separate supply means be.

One further preventing leakage of chalcogen vapor from one Evaporation chamber in a feeder can by a Carrier gas feed into the pipeline between valve and evaporation chamber can be realized. The flow velocity This carrier gas feed can, for example, over detected a flow meter and adjusted via a fine regulating become.

In An embodiment of the invention are components that with the Chalcogen vapor or the chalcogen vapor / carrier gas mixture can be contacted preferably from a relative to this Mixture resistant material, such as graphite.

Farther Components that come in contact with chalcogen vapor should be heated so that condensation of the chalcogen on these components is prevented. This prevents a complicated cleaning and maintenance.

A Possibility to realize this, parts of the device in a block, for example made of graphite, accommodate and this with an integrated heater to the desired temperature too heat.

In a further development of the invention are the openings for the supply and discharge of the chalcogen vapor / carrier gas mixture, the evaporation chambers including the connecting pipes in a vapor deposition head, which is in a recess in the transport opposite wall is used, ie above the Substrates, housed.

Of the Evaporation head is preferably made of a material which is resistant against the chalcogen vapor is, in particular, for example Graphite.

Of the Evaporator head can, for example, via an integrated heating, be brought to a desired temperature.

Farther can be a thermal decoupling of the evaporation head of the process chamber be provided. This allows, for example, the vapor deposition head at high temperatures, whereas, for example, the means of transport can be tempered to low temperatures.

In a further development of the invention, the vapor deposition head under a sealed hood with integrated cooling system provided become. The interior of the hood can be in a special design with a protective gas are flooded and sucked off.

In a continuation of the invention are further components come into contact with chalcogen vapor, for example, the evaporation chambers and the pipes between the evaporation chamber and the opening for feeding the chalcogen vapor / carrier gas mixture, As well as nitrogen gas feeds housed in the Aufdampfkopf. The Accommodating the nitrogen gas feeds in the evaporation head has the advantage that already nitrogen gas in the evaporation head heated.

One Embodiment of the invention will be described with reference to the attached Drawings explained.

It shows:

1 an overview of a device for coating substrates with chalcogens,

2 a process chamber with input and output gas locks,

3 an evaporation head and

4 a schematic drawing of a selenium feed device.

1 shows an overview of a device for coating substrates, such as pre-prepared glass substrates, with chalcogens. The following is based on a coating with selenium. So that, for example, toxic selenium dioxide can not arise, the entire process must take place in a defined atmosphere, in particular with the exclusion of oxygen. For example, nitrogen may be used as the protective / carrier gas.

This is partly due to a housing 1 , which consists of a box of Plexiglas, or other suitable material, and a housing exhaust 2 guaranteed. The housing 1 has two opposite openings 1.1 . 1.2 (see arrows) for introducing and carrying out the substrates, not shown, by means of a means of transport 3 , The openings 1.1 . 1.2 in the case 1 define a subspace of the housing 1 enclosed space and indeed a transport channel 4 ,

A central part of the transport channel 4 defines a process chamber 5 , This process chamber 5 is surrounded by walls and also has two opposite openings 5.1 . 5.2 (see arrows) through which the transport channel 4 goes through it. These openings 5.1 . 5.2 allow substrates using the means of transport 3 through the transport channel 4 in the process chamber 5 to transport in and out. The substrates are transported at a constant speed.

2 shows that the two openings 5.1 . 5.2 the process chamber 5 with an input side 6 and exit gas lock 7 are provided. Every gas lock 6 . 7 consists of two gas curtains made of nitrogen, which in 2 are indicated by arrows. The nitrogen gas of the respective outer gas curtains is sucked through a housing exhaust to the outside, the nitrogen gas of the respective inner Gasvor hang is via an exhaust in the process chamber 5 inside, into the process chamber 5 into it, sucked.

The gas locks 6 . 7 allow the system to operate in a continuous process, at atmospheric pressure and under defined residual gas conditions, in particular with the exclusion of oxygen.

The actual coating of the substrates takes place in the region of a recess 8th that are in the means of transport 3 opposite wall of the process chamber 5 is held. This will be a in 3 detailed vapor deposition head 9 , in this recess 8th used, cf. also 1 , The evaporation head 9 is a block of graphite with cutouts.

For further protection, so that no selenium can escape into the environment, is the Aufdampfkopf 9 under a tight hood 10 ( 1 ) provided with an integrated cooling system, not shown. The space between the hood 10 and the evaporation head 9 can be flooded with nitrogen, or rinsed and sucked off.

A Selendampf- / nitrogen gas mixture is via a slit-shaped opening 11 in the evaporation head 9 , which is aligned perpendicular to the transport direction of the substrates, in the process chamber 5 brought in. An extraction via another slot-shaped opening 12 parallel to the slit-shaped opening 11 aligned to supply the Selendampf- / nitrogen gas mixture and is offset to this in the transport direction of the substrates, leads to a flow of selenium vapor / carrier gas mixture along the transport channel 4 in the process chamber 5 , In the area of the process chamber 5 through the two openings 11 . 12 is limited, the actual coating of the substrates takes place. This zone is therefore also called coating zone.

The plant is operated so that the Selendampf- / carrier gas mixture in the transport direction ( 2 ) of the substrates flows.

Around a uniform coating of the substrates vertically to get to the transport direction, the selenium vapor over the entire width of the substrate applied evenly become. A homogeneous distribution can be used for further process steps be decisive.

For this purpose, a line on the Selendampf- / carrier gas mixture of the slot-shaped opening 11 supplied in the lower part of the shape of the slot-shaped opening.

The homogeneous distribution is over a slot 13 for supplying the Selendampf- / carrier gas mixture with several successive constrictions and extensions in the Aufdampfkopf 9 realized ( 3 ). The slot 13 to Zufüh tion runs parallel to the slot-shaped opening 11 and ends at this opening. The mixture accumulates in a constriction and can then expand again in a relaxation zone. This process is repeated several times. As a result, the selenium vapor / carrier gas mixture is distributed uniformly over the entire slot-shaped opening 13 time.

Furthermore, the wall has the process chamber 5 between the slot-shaped opening 11 to the feeder and the slot-shaped opening 12 for discharging a wave-like surface with wave crests perpendicular to the transport direction of the sub strate. As a result, better mixing of the chalcogen vapor / carrier gas mixture conducted over the surface of the substrates is achieved.

The selenium that in the coating zone between the slots 11 . 12 not condensed on the substrates, is combined with the nitrogen over the slit-shaped opening 12 for suction and then over a slot 14 for suction, which is parallel to the slot-shaped opening 12 extends to the suction and ends at this opening, from the process chamber 5 out and then over a slightly downwardly inclined exhaust pipe 15 dissipated. The slot 12 for suction and the exhaust pipe 15 can together as an exhaust pipe leading to the slot-shaped opening 14 towards the shape of the slot-shaped opening 12 assumes to be viewed. The slot 12 for suction is also provided with several constrictions and extensions. This allows a uniform extraction of the excess selenium vapor / carrier gas mixture over the entire width.

4 shows a schematic drawing of a selenium feed device.

Selenium is commercially available spherically in solid state. The balls have a diameter of about 3 mm. The selenkugeln are placed in a funnel-shaped container 16 poured and stored there. The funnel-shaped container 16 has at its lower end an opening through which the selenkalls vertically down into a metering device located underneath 17 can fall. In addition, the funnel-shaped container 16 equipped with a level gauge.

The dosing device 17 consists of a cylindrical housing and a centrally rotatably mounted therein, also cylindrical rotary member, hereinafter referred to as drum. The housing has two holes, one on the top and one on the bottom on the same pitch diameter and offset in their position by 180 °. The inner rotary part has four holes, which lie on the same pitch circle diameter. In their length, the two parts are designed so that no selenium ball fits between them.

Lie the holes of the parts aligned over each other, can the selenium balls fall into the drum. If the drum is rotated by 90 °, the selenium balls can move the drum and the casing, vertically falling down, left.

about the amount of time that passes between the 90 ° turns and the number of selenium balls entering the bore of the drum fit, the number of selenium balls and so on dose the amount of selenium provided.

Subsequently, the selenium balls fall through a substantially vertical pipeline 18 in a heated chamber 19 , also called evaporation chamber. In the vertical pipeline 18 is a, designed as a ball valve with full opening, valve 20 installed, which is opened only during the period of dosing. As a result, virtually no vapor can escape from the heated chamber, in which selenium vapor is present, into the supply device.

Further preventing the escape of selenium vapor from the vaporization chamber 19 into the feeder via the pipeline 18 from the metering device 17 or from the container 16 is through a nitrogen gas feed into the pipeline 21 between valve 20 and evaporation chamber 19 realized. This flow of nitrogen creates a flow into the vaporization chamber 19 into it and prevents a flow in the opposite direction.

As described, the selenium balls fall from above into the chamber 19 , The chamber 19 is a simple horizontal hole or hole in a block of graphite, ie in the vapor deposition head 9 ( 3 ), and is closed at both ends. In this chamber 19 which in addition to selenium supply via the line 18 an entrance 22 and an exit 23 possesses, selenium collects. The mentioned inputs and outputs 22 . 23 are located on the upper side of the hole.

The block, ie the evaporation head 9 , is heated together with the selenium via a heater, not shown. By heating, the selenium is first melted and then evaporates at a further temperature rise. In the lower part of the chamber is then a liquid Selensee 24 , and in the upper part Selendampf 25 ,

To the level in the chamber 19 To regulate, an unillustrated level sensor is provided. The level sensor indicates to the beschrie bene dosing a signal when too few selenium in the chamber 19 is. Thereafter, the process begins, so that selenium falls into the chamber. If a sufficient level is reached, the level sensor stops the dosing process via a signal.

The selenium vapor that has formed in the chamber must now be led to the substrate. It must be ensured that the selenium vapor can neither cool nor condense. The transport of the vapor takes place via a carrier gas. Nitrogen is used as the carrier gas. This must first be heated to the same temperature as prevails in the chamber. The nitrogen passes through the entrance 22 in the chamber 19 in which the selenium vapor is located. There, the selenium vapor is added and as Selendampf- / nitrogen mixture through the output 23 the chamber 19 transported in the direction of the substrate. The pipe between the chamber and the slot-shaped opening 13 The feed must also be heated to prevent condensation of selenium, which would require extensive maintenance.

In order to facilitate this preheating of the nitrogen gas, the heating of the vaporization chamber and the transport routes, everything is in the vapor deposition head 9 housed in graphite. The whole steam head 9 is heated. The nitrogen gas is passed through a meander, not shown, in the vapor deposition head 9 carried out. The gas heats up to the temperature of the vapor deposition head 9 ,

In addition, the flow of the selenium vapor mixed nitrogen gas over another, in the line between the evaporation chamber and slit-like opening 11 to the feeder 11 located nitrogen gas feed 26 controlled. The inflow of this gas, called process additive gas, a slight suction is developed, the gas mixture from the chamber 19 draws. The flow through the nitrogen gas feed for the process additive gas can be measured via a flow meter and adjusted via a fine adjustment valve.

To the flow rate of the nitrogen feed for the process additive gas 26 , the nitrogen feed into the pipeline 21 and the nitrogen feed into the vaporization chamber 22 These are each equipped with a flow meter and a fine regulating valve. This allows the corresponding rivers to be measured and then adjusted.

in the In the above embodiment, selenium stands for the other chalcogens except oxygen.

1

casing

1.1

opening

1.2

opening

2

housing suction

3

Mode of Transport

4

transport channel

5

process chamber

5.1

opening

5.2

opening

6

input-side gas lock

7

Load-side gas lock

8th

recess

9

Aufdampfkopf

10

Hood

11

Slot-shaped opening to the feeder

12

Slot-shaped opening for suction

13

slot to the feeder

14

slot for suction

15

exhaust pipe

16

container

17

metering

18

pipeline

19

chamber

20

Valve

21

Nitrogen gas feed into the pipeline

22

entrance

23

output

24

Selensee

25

selenium vapor

26

Nitrogen gas feed for the process additive gas

QUOTES INCLUDE IN THE DESCRIPTION

This list The documents listed by the applicant have been automated generated and is solely for better information recorded by the reader. The list is not part of the German Patent or utility model application. The DPMA takes over no liability for any errors or omissions.

Cited patent literature

• - EP 2008/007466 [0004]
• - DE 102004024601 [0008]
• - EP 2008/062061 [0009]

Claims (23)

Process for coating flat substrates with chalcogens in the form of thin layers in a process chamber, characterized by - forming an inlet and outlet gas lock ( 6 . 7 ) for the oxygen-tight closure of the process chamber ( 5 ), - introducing one or more substrates to be coated and tempered to a predetermined temperature in a transport direction into the process chamber ( 5 ), - introducing a uniformly distributed over the width of the substrates chalcogen vapor / carrier gas mixture in the one transport channel ( 4 ) having process chamber ( 5 ) above the substrates, - forming a flow of the chalcogen vapor / carrier gas mixture over the substrates through the transport channel ( 4 ) between the input and output side gas locks ( 6 . 7 ), - forming a chalcogen layer on the substrates by means of PVD during a predetermined residence time in the process chamber ( 5 ) and - removing the excess chalcogen vapor not condensed on the substrates and the carrier gas between the gas locks ( 6 . 7 ), and - removal of the substrates from the process chamber ( 5 ) after a predetermined residence time has elapsed. A method according to claim 1, characterized in that the chalcogen vapor / carrier gas mixture after introduction into the process chamber ( 5 ) above the substrates along the transport channel ( 4 ) flows in the transport direction and then removed again. A method according to claim 1, characterized in that the chalcogen vapor / carrier gas mixture after introduction into the process chamber ( 5 ) above the substrates along the transport channel ( 4 ) flows against the transport direction and is then removed again. Method according to one of claims 1 to 3, characterized in that the substrates prior to introduction into the process chamber ( 5 ) to a temperature of below 200 ° C, preferably room temperature, tempered. Method according to one of the preceding claims, characterized in that the substrates during the Coating to a temperature of less than 200 ° C, preferably between 20 ° C and 100 ° C, tempered. Apparatus for coating flat substrates with chalcogens in the form of thin layers in a process chamber, which is provided with an opening for introducing the substrates and with an opening for discharging the substrates, and an inlet-side gas lock at the opening for introducing the substrates and an output side Gas lock at the opening for discharging the substrates, and which is provided with a transport means for the flat substrates through the process chamber, characterized in that in the transport means opposite wall of the process chamber ( 5 ) between the gas locks ( 6 . 7 ) an opening ( 11 ) for supplying a chalcogen vapor / carrier gas mixture and laterally offset to an opening ( 12 ) are present for the removal of the chalcogen vapor / carrier gas mixture. Apparatus according to claim 6, characterized in that a further to the other two openings ( 11 . 12 ) laterally offset opening in the transport-opposite wall for supplying a chalcogen vapor / carrier gas mixture is present, wherein the openings in the order feeding, discharge and supply along the process chamber ( 5 ) are arranged. Apparatus according to claim 6 or 7, characterized in that a housing ( 1 ) the process chamber ( 5 ) and with two opposite openings ( 1.1 . 1.2 ) and a transport channel ( 4 ) is provided between, passing through the process chamber ( 5 ). Apparatus according to claim 8, characterized in that the housing ( 1 ) has a suction. Device according to one of claims 6 to 9, characterized in that the gas locks ( 6 . 7 ) each consist of at least two gas curtains. Apparatus according to claim 10, characterized in that between the gas curtains of the gas locks ( 6 . 7 ), a suction is present. Device according to one of claims 6 to 11, characterized in that the device is a tempering device for tempering the substrates to a temperature below 200 ° C provides. Device according to one of claims 6 to 12, characterized in that the openings ( 11 . 12 ) are slot-shaped openings which are aligned perpendicular to the transport direction and in each case over the entire width of the in the process chamber ( 5 ) extend substrates. Apparatus according to claim 13, characterized in that the wall of the process chamber ( 5 ) over the substrates between the slot-shaped ones gene openings ( 11 ) to the feed and the slot-shaped opening ( 12 ) For discharging a wave-like surface with wave crests perpendicular to the transport direction of the substrates. Device according to one of claims 6 to 14, characterized in that each opening for supplying a chalcogen vapor / carrier gas mixture via at least one line with an evaporation chamber ( 19 ) connected is. Apparatus according to claim 15, characterized in that the lines to a slot-shaped opening ( 11 ; 12 ), in the lower part the shape of the slot-shaped opening ( 11 ; 12 ) and are provided with constrictions followed by relaxation zones. Apparatus according to claim 15 or 16, characterized in that the evaporation chambers ( 19 ) each with at least one feed device, consisting of a container ( 16 ) and a metering device ( 17 ), via pipelines with valves ( 20 ) are connected. Device according to one of claims 15 to 17, characterized in that between the evaporation chambers ( 19 ) and the respective opening ( 11 ) for supplying the chalcogen vapor / carrier gas mixture, an additional carrier gas feed ( 26 ) is available. Apparatus according to claim 18, characterized in that a flow divider with the opening ( 12 ) is connected to the suction of the chalcogen vapor / carrier gas mixture, wherein an output of the flow divider with the additional carrier gas feed ( 26 ) connected is. Device according to one of claims 6 to 19, characterized in that the openings ( 11 . 12 ) for the supply and discharge of the chalcogen vapor / carrier gas mixture, the evaporation chambers ( 19 ) including the connecting lines in a vapor deposition head ( 9 ) are housed in a recess ( 8th ) in the transport chamber opposite wall of the process chamber ( 5 ) is used. Apparatus according to claim 20, characterized in that the vapor deposition head ( 9 ) is provided with a heater. Apparatus according to claim 20 and 21, characterized in that the vapor deposition head ( 9 ) under a tight hood ( 10 ) is provided with integrated cooling system. Device according to claim 22, characterized in that the space between the hood ( 10 ) and the vapor deposition head ( 9 ) can be flooded with a protective gas and sucked.