Temperature-controlled gas supply line with dilution gas flows supplied at multiple locations
10472718 ยท 2019-11-12
Assignee
Inventors
- Markus Gersdorff (Herzogenrath, DE)
- Martin DAUELSBERG (Aachen, DE)
- Baskar Pagadala Gopi (Aachen, DE)
- Michael LONG (Herzogenrath, DE)
Cpc classification
C23C16/45561
CHEMISTRY; METALLURGY
C23C16/4481
CHEMISTRY; METALLURGY
C23C16/52
CHEMISTRY; METALLURGY
International classification
C23C16/455
CHEMISTRY; METALLURGY
C23C14/54
CHEMISTRY; METALLURGY
C23C16/52
CHEMISTRY; METALLURGY
C23C16/448
CHEMISTRY; METALLURGY
Abstract
A device and a method for depositing organic layers onto a substrate includes a process gas source with a temperature-controlled evaporator, and a carrier gas supply line which opens into the evaporator in order to supply a carrier gas flow into a temperature-controlled first transport line. A first dilution gas supply line, which opens into the first transport line, supplies a dilution gas flow into the first transport line. The device also comprises a temperature-controlled gas inlet element fluidly connected to the first transport line. A gaseous starting material can be supplied into a processing chamber via the gas inlet element. A substrate is disposed on a temperature-controlled susceptor located in the processing chamber, and a layer is grown on the substrate using the gaseous starting material.
Claims
1. A device for depositing one or more organic layers onto a substrate (20), the device comprising: a first process gas source (1) with a first evaporator (1), wherein a first solid or liquid starting material is evaporated into a first gaseous starting material in the first evaporator (1), wherein the first process gas source (1) is temperature-controlled to a first source temperature (T.sub.1) by a first source temperature-controlling device (2); a first carrier gas supply line (4) fluidly connected to the first evaporator (1) and configured to feed a first carrier gas flow for transporting the first gaseous starting material out of the first evaporator (1) into a first transport line (5); the first transport line (5) that is temperature-controlled to a first line temperature (T.sub.2) by means of a line temperature-controlling device (7); a first dilution gas supply line (8) fluidly connected to the first transport line (5) and configured to feed a first dilution gas flow into the first transport line (5), wherein the first dilution gas supply line (8) is located upstream from the first line temperature-controlling device (7); a processing chamber (30); a gas inlet element (31) disposed in the processing chamber (30) and configured to supply the first gaseous starting material into the processing chamber (30), wherein the gas inlet element (31) is temperature-controlled to a gas inlet temperature (T.sub.5) by means of a gas inlet temperature-controlling device (32), wherein the gas inlet element (31) is fluidly connected to the first transport line (5); a second dilution gas supply line (34) fluidly connected to the gas inlet element (31) upstream from the gas inlet temperature-controlling device (32) and configured to feed a second dilution gas flow into the gas inlet element (31); a susceptor (35) that is temperature-controlled to a susceptor temperature (T.sub.6) by means of a susceptor temperature-controlling device (37), wherein the substrate (20) is disposed on the susceptor (35), and wherein a layer is grown on the substrate (20) by means of the first gaseous starting material; and a controlling device (38) configured to control the first source temperature-controlling device (2) such that a temperature of the first source temperature-controlling device (2) is equal to the first source temperature (T.sub.1), configured to control the first line temperature-controlling device (7) such that a temperature of the first line temperature-controlling device (7) is equal to the first line temperature (T.sub.2), configured to control the gas inlet temperature-controlling device (32) such that a temperature of the gas inlet temperature-controlling device (32) is equal to the gas inlet temperature (T.sub.5), and configured to control the susceptor temperature-controlling device (37) such that a temperature of the susceptor temperature-controlling device (37) is equal to the susceptor temperature (T.sub.6), wherein the controlling device (38) is further configured to, while the layer is being deposited on the substrate (20), control the first source temperature (T.sub.1) to be higher than the first line temperature (T.sub.2), control the first line temperature (T.sub.2) to be higher than the gas inlet temperature (T.sub.5), and control the gas inlet temperature (T.sub.5) to be higher than the susceptor temperature (T.sub.6).
2. The device of claim 1, further comprising: a second process gas source (11) with a second evaporator (11), wherein a second solid or liquid starting material is evaporated into a second gaseous starting material in the second evaporator (11), and wherein the second process gas source (11) is temperature controlled to a second source temperature (T.sub.1) by a second temperature-controlling device (12); a second carrier gas supply line (14) fluidly connected to the second evaporator (11) and configured to feed a second carrier gas flow for transporting the second gaseous starting material out of the second evaporator (11) into a second transport line (15), wherein the second transport line (15) is temperature-controlled to a second line temperature (T.sub.2) by means of a second line temperature-controlling device (17); a third dilution gas supply line (18) fluidly connected to the second transport line (15), through which a third dilution gas flow is fed into the second transport line (15) wherein the first transport line (5) and second transport line (15) are fluidly connected to a mixing device (21), which is temperature-controlled to a mixer temperature (T.sub.3) by means of a mixer temperature-controlling device (22); and, a fourth dilution gas supply line (24) fluidly connected to the mixing device (21) upstream from the mixer temperature-controlling device (22), and configured to feed a fourth dilution gas flow into the mixing device (21).
3. The device of claim 2, wherein the mixer temperature (T.sub.3) is lower than both the first and second line temperatures (T.sub.2, T.sub.2), and higher than the gas inlet temperature (T.sub.5).
4. The device of claim 2, further comprising: a third transport line (25) located downstream from the mixing device (21) and upstream from the gas inlet element (31), wherein the third transport line (25) is configured to transport the first and second gaseous starting materials from the mixing device (21) into the gas inlet element (31), wherein the third transport line (25) is temperature-controlled to a third line temperature (T.sub.4) by a third line temperature-controlling device (27; and a fifth dilution gas supply line (28) fluidly connected to the third transport line (25) upstream from the third line temperature-controlling device (27) and configured to feed a fifth dilution gas flow into the third transport line (25).
5. The device of claim 4, wherein the mixer temperature (T.sub.3) is higher than the third line temperature (T.sub.4), and the third line temperature (T.sub.4) is higher than the gas inlet temperature (T.sub.5).
6. A method for depositing one or more organic layers onto at least one substrate (20), the method comprising: evaporating, in a first evaporator (1) of a first process gas source (1), a first solid or liquid starting material into a first gaseous starting material, wherein the first process gas source (1) is temperature-controlled to a first source temperature (T.sub.1) by a first source temperature-controlling device (2); feeding, by a first carrier gas supply line (4), a first carrier gas into the first evaporator (1), wherein the first carrier gas transports the first gaseous starting material out of the first evaporator (1) into a first transport line (5), wherein the first transport line (5) is temperature-controlled to a first line temperature (T.sub.2) by means of a first line temperature-controlling device (7); feeding, by a first dilution gas supply line (8), a first dilution gas flow into the first transport line (5), wherein the first dilution gas supply line (8) is located upstream from the first line temperature-controlling device (7); supplying, by a gas inlet element (31), the first gaseous starting material into a process chamber (30), wherein the gas inlet element (31) is temperature-controlled to a gas inlet temperature (T.sub.5) by means of a gas inlet temperature-controlling device (32), and is fluidly connected to the first transport line (5); feeding, by a second dilution gas supply line (34), a second dilution gas flow into the gas inlet element (31) upstream from the gas inlet temperature-controlling device (32); and depositing a layer on the at least one substrate (20) lying on a susceptor (35) by means of the gaseous starting material, wherein the susceptor is disposed in the process chamber (30) and is temperature-controlled to a susceptor temperature (T.sub.6) by means of a susceptor temperature-controlling device (37), wherein, while depositing the layer, the first source temperature (T.sub.1) is higher than the first line temperature (T.sub.2) the first line temperature (T.sub.2) is higher than the gas inlet temperature (T.sub.5), and the gas inlet temperature (T.sub.5) is higher than the susceptor temperature (T.sub.6).
7. The method of claim 6, further comprising: evaporating, in a second evaporator (11) of a second process gas source (11), a second a solid or liquid starting material into a second gaseous starting material, wherein the second process gas source (11) is temperature-controlled to a second source temperature (T.sub.1) by means of a second source temperature-controlling device (12); feeding, by a second carrier gas supply line (14), the second carrier gas into the second evaporator (11), wherein the second carrier gas transports the second gaseous starting material out of the second evaporator (11) into a second transport line (15), wherein the second transport line (15) is temperature-controlled to a second line temperature (T.sub.2) by means of a second line temperature-controlling device (17); feeding, by a third dilution gas supply line (18), a third dilution gas flow into the second transport line (15), wherein the first transport line (5) and second transport line (15) are fluidly connected to a mixing device (21), which is temperature-controlled to a mixer temperature (T.sub.3) by means of a mixer temperature-controlling device (22); and, feeding, by a fourth dilution gas supply line (24), a fourth dilution gas flow into the mixing device (21) upstream from the mixer temperature-controlling device (22).
8. The method of claim 7, wherein the mixer temperature (T.sub.3) is lower than both the first and second line temperatures (T.sub.2, T.sub.2), and higher than the gas inlet temperature (T.sub.5).
9. The method of claim 7, further comprising: transporting, by a third transport line (25), the first and second gaseous starting materials from the mixing device (21) to the gas inlet element (31), wherein the third transport line (25) is temperature-controlled to a third line temperature (T.sub.4) by a third line temperature-controlling device (27); and feeding, by a fifth dilution gas supply line (28), a fifth dilution gas flow into the third transport line (25) upstream from the third line temperature-controlling device (27).
10. The method of claim 9, wherein the mixer temperature (T.sub.3) is higher than the third line temperature (T.sub.4), and the third line temperature (T.sub.4) is higher than the gas inlet temperature (T.sub.5).
11. The method of claim 6, wherein a partial pressure of the first gaseous starting material in the first carrier gas is incrementally diminished between the first evaporator (1) and the gas inlet element (31) at different points spaced apart from each other in a direction of flow of the first gaseous starting material, wherein the temperature in the flow of the first gaseous starting material at each point between the first evaporator (1) and the gas inlet element (31) is higher than a condensation temperature of the gaseous starting material.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1) An exemplary embodiment of the invention will be explained below based on the attached drawings. Shown on:
(2)
(3)
(4)
DETAILED DESCRIPTION
(5) The device illustrated only schematically on
(6) The process gas contains a gaseous starting material, which is fed into the processing chamber 30. The temperature of the surface of the substrate 20 is lower than the condensation temperature of the gaseous starting material, so that the gaseous starting material condenses on the upper side of the substrate 20 as a layer.
(7) Provided within the gas inlet element 31 is a temperature-controlling device 32. This temperature-controlling device 32 is designed as a heater in the exemplary embodiment, and used to adjust the temperature of the gaseous starting material to the temperature T.sub.5 (gas inlet temperature).
(8) The device has at least one source 1, in which a solid or liquid starting material 3 is held available. The starting material 3 is kept at a source temperature T.sub.1, which is higher than the gas inlet temperature T.sub.5. The starting material 3 can be stored as a porous body, a powder or the like. However, the starting material can also be coated onto a porous body. A source temperature-controlling device 2 is provided that takes the form of a heater. The heater continually feeds heat into an evaporator 1, which contains the starting material 3, so that the starting material 3 is converted into gaseous form. However, a liquid starting material can also be used in place of a solid starting material.
(9) A carrier gas supply line 4 opens into the evaporator 1. A mass flow controller 41 is used to feed a carrier gas flow into the evaporator 1 . Involved here is argon, nitrogen, hydrogen or another inert gas. The starting material 3 converted into gaseous form is transported from the evaporator 1 through a gas outlet 6. The gas outlet 6 is connected with a transport line 5, so that the gaseous starting material can be fed out of the gas outlet 6 and into the transport line 5. Immediately downstream from the gas outlet 6, a dilution gas supply line 8 opens into the adjoining transport line 5. A dilution gas is fed into the gas line through the dilution gas supply line 8. The mass flow of the gas fed into the carrier gas supply line and the mass flow of the gas fed into the dilution gas line is regulated by a mass flow controller 41, 42, respectively. The carrier gas flow that transports the gaseous starting material is thereby mixed with the dilution gas flow at the feed-in point 9, wherein the dilution gas is the same gas also comprising the carrier gas flow.
(10) The transport line 5 adjoining the feed-in point 9 is heated by a heating device 7. This line temperature-controlling device is designed as a heating sleeve. It heats the transport line 5 to a transport line temperature T.sub.2 that is lower than the source temperature T.sub.1.
(11) Provided in the exemplary embodiment is a second process gas source 11, which exhibits a second evaporator 11 that is also provided with a heating device 12, with which a liquid or solid starting material 13 is adjusted to a second source temperature T.sub.1. Here as well, a supply line 14 opens into the evaporator 11, and carries a carrier gas flow controlled by means of a mass flowmeter 43, feeding it into the evaporator 11. The carrier gas transports the evaporated starting material out of the evaporator 11 through a gas outlet 16.
(12) A dilution gas is fed into the gas flow at a feed-in point 19. This takes place by means of a dilution gas supply line 18, through which a mass flow of a dilution gas controlled by a mass flow controller 44 is supplied.
(13) Extending downstream from the feed-in point 19 is a transport line 15, which is enveloped by a heating sleeve that comprises a line heater 17, with which the transport line 15 is kept at a line temperature T.sub.2. The line temperature T.sub.2 is lower than the source temperature T.sub.1. The starting material 13 consists of various organic materials.
(14) The transport line 5 and transport line 15 open into a mixing device 21, which incorporates gas deflection elements 23 used to mix together the gas mixtures entering into the mixing device 21 from the transport lines 5, 15.
(15) Provided inside of the mixing device 21 is a mixing temperature-controlling device 22. Involved here is a heating device, with which the mixing device 21 and in particular the gas deflection elements 23 are kept at a mixer temperature T.sub.3. The mixer temperature T.sub.3 is lower than the line temperatures T.sub.2, T.sub.2. In order to prevent the gaseous starting material from condensing on the gas deflection surfaces 23, the gas mixture comprised of carrier gas and gaseous starting material that enters into the mixing device 21 is diluted further. To this end, another dilution gas supply line 24 opens into the mixing chamber of the mixer 21 upstream from the gas deflection elements 23 and in particular upstream from the heating device 22. The dilution gas flow fed into the mixing chamber through the dilution gas supply line 24 is controlled by a mass flow controller 45.
(16) The gas mixture mixed in the mixing device 21 exits the mixing device 21 through a gas outlet 26. Located there is another feed-in point 29, at which another dilution gas supply line 28 opens into the gas flow. Another dilution gas flow controlled by a mass flow regulator 46 is fed into the gas flow through the dilution gas supply line 28. The feed-in point 29 is located immediately downstream from the gas outlet 26.
(17) The transport line 25 extending downstream from the feed-in point 29 is heated by a heating sleeve 27 to a line temperature T.sub.4 that is lower than the mixer temperature T.sub.3 and higher than the temperature T.sub.5 inside of the gas inlet element 31.
(18) The transport line 25 opens into the gas inlet element 31, in which a heating device 32 is located. Upstream from the heating device 32, a dilution gas supply line 34 opens into the gas inlet element 31, through which another dilution gas flow controlled by a mass flow regulator 47 is fed into the gas inlet element 31. The gas flow fed into the gas inlet element 31 is thereby diluted further upstream from the heating device 32.
(19) The incremental dilution of the gaseous starting material in the gas line between the source 1, 11 or evaporator 1, 11 and gas inlet element 31 leads to an incremental reduction in the partial pressure of the gaseous starting material or gaseous starting material inside of the gas line system in the direction of flow. This enables the temperature progression described above in the gas transport system as illustrated on
(20)
(21) The above statements serve to explain the inventions encompassed by the application as a whole, which each separately further develop the prior art at least through the following feature combinations:
(22) A device, characterized in that the first dilution gas supply line 8, 18 is situated upstream from the line temperature-controlling device 7, 17, and another dilution gas supply line 34 opens into the gas inlet element 31 upstream from the gas inlet temperature-controlling device 32, so as to feed a dilution gas flow into the gas inlet element 31.
(23) A device, characterized by a controlling device set up so as to be able to adjust the source temperature-controlling device 2, 12 to the source temperature T.sub.1, T.sub.1, the line temperature-controlling device 7, 17 to the line temperature, T.sub.2, T.sub.2, the gas inlet temperature-controlling device 32 to the gas inlet temperature T.sub.5, and the susceptor temperature-controlling device 37 to the susceptor temperature T.sub.6.
(24) A method, characterized in that the first dilution gas supply line 8, 18 is situated upstream from the line temperature-controlling device 7, 17, and that a dilution gas flow is fed into the gas inlet element 31 through another dilution gas supply line 34, which opens into the gas inlet element 31 upstream from the gas inlet temperature-controlling device 32.
(25) A device, characterized in that the first source temperature T.sub.1, T.sub.1 is higher than the line temperature T.sub.2, T.sub.2, the line temperature T.sub.2, T.sub.2 is higher than the gas inlet temperature T.sub.5, and the gas inlet temperature T.sub.5 is higher than the one susceptor temperature T.sub.6.
(26) A device, characterized by a process gas source that exhibits a second evaporator 11, wherein a solid or liquid second starting material can be evaporated into a second gaseous starting material at a second source temperature T.sub.1 in the second evaporator 11 by supplying heat generated by a second source temperature-controlling device 12, wherein a second carrier gas supply line 14 opens into the second evaporator 11 for supplying a second carrier gas flow to transport the second gaseous starting material out of the second evaporator 11 and into a second transport line 15, wherein the second transport line 15 is temperature-controlled to a second line temperature T.sub.2 by a second line temperature-controlling device 17, and a second dilution gas supply line 18 opens into the second transport line 15, through which a second dilution gas flow is fed into the second transport line 18, wherein the first transport line 8 and second transport line 18 open into a mixer 21, which is temperature-controlled to a mixer temperature T.sub.3 by a mixer temperature-controlling device 22, wherein a dilution gas supply line 24 opens into the mixing device 21 upstream from the mixer temperature-controlling device 22, and is used to feed a dilution gas flow into the mixing device 21.
(27) A method, characterized by a process gas source that exhibits a second evaporator 11, wherein a solid or liquid second starting material is evaporated into a second gaseous starting material at a second source temperature T.sub.1 in the second evaporator 11 by supplying heat generated by a second source temperature-controlling device 12, wherein a second carrier gas supply line 14 opens into the second evaporator 11, into which is fed a second carrier gas flow that transports the second gaseous starting material out of the second evaporator 11 and into a second transport linen 15, wherein the second transport line 15 is temperature-controlled to a second line temperature T.sub.2 by a second line temperature-controlling device 17, and a second dilution gas supply line 18 opens into the second transport line 15, through which a second dilution gas flow is fed into the second transport line 18, wherein the first transport line 8 and second transport line 18 open into a mixer 21, which is temperature-controlled to a mixer temperature T.sub.3 by a mixer temperature-controlling device 22, wherein a dilution gas supply line 24 opens into the mixing device 21 upstream from the mixer temperature-controlling device 22, and is used to feed a dilution gas flow into the mixing device 21.
(28) A device, characterized in that the mixer temperature T.sub.3 is lower than the first and second line temperature T.sub.2, T.sub.2, and higher than the gas inlet temperature T.sub.5.
(29) A device, characterized by a transport line 25 situated downstream from the mixing device 21 and upstream from the gas inlet element 31 for transporting the gaseous starting material from the mixing device 21 into the gas inlet element 31, which can be temperature-controlled to a line temperature T.sub.4 by a line temperature-controlling device 27, wherein a dilution gas supply line 28 opens into the transport line 25 upstream from the line temperature-controlling device 27 to feed a dilution gas flow into the transport line 25.
(30) A method, characterized by a transport line 25 situated downstream from the mixing device 21 and upstream from the gas inlet element 31 through which the gaseous starting material is transported from the mixing device 21 into the gas inlet element 31, which is temperature-controlled to a line temperature T.sub.4 by a line temperature-controlling device 27, wherein a dilution gas supply line 28 opens into the transport line 25 upstream from the line temperature-controlling device 27, with which the a dilution gas flow is fed into the transport line 25.
(31) A device, characterized in that the mixer temperature T.sub.3 is higher than the line temperature T.sub.4, and the line temperature T.sub.4 is higher than the gas inlet temperature T.sub.5.
(32) A method, characterized in that the partial pressure of the gaseous starting material in the carrier gas flow is incrementally diminished by feeding a plurality of dilution gas flows into a heated line connection between the evaporator 1, 11 and gas inlet element 31 at different points spaced apart from each other in the direction of flow, wherein the line connection is heated in such a way that the temperature in the gas flow is higher than the condensation temperature of the gaseous starting material at each point on the line connection.
(33) All disclosed features are essential to the invention (taken individually, but also in combination with each other). The disclosure of the application hereby also incorporates the disclosure content of the accompanying/attached priority documents (copy of prior application) in its entirety, also for the purpose of including features in these documents in claims of the present application. The features in the subclaims characterize independent inventive further developments of prior art, in particular with the aim of implementing partial applications based upon these claims.
REFERENCE LIST
(34) TABLE-US-00001 1 Process gas source 1 Evaporator 2 Heating device T.sub.1 3 Starting material 4 Supply line 1 5 Transport line 6 Gas outlet 7 Heating device T.sub.2 8 Supply line 9 Feed-in point 10 CVD reactor 11 Process gas source 11 Evaporator 12 Heating device T.sub.1 13 Starting material 14 Supply line 15 Transport line 16 Gas outlet 17 Heating device T.sub.2 18 Supply line 19 Feed-in point 20 Substrate 21 Mixing device 22 Heating device T.sub.3 23 Gas deflection element 24 Supply line 25 Transport line 26 Gas outlet 27 Temperature-controlling device, cooling device T.sub.4 28 Supply line 29 Feed-in point 30 Processing chamber 31 Gas inlet element 32 Heating device T.sub.5 33 Gas outlet opening 34 Supply line 35 Susceptor 36 Discharge line 37 Cooling device T.sub.6 38 Controlling device 39 40 41 Mass flow controller Line 1 42 Mass flow controller Line 2 43 Mass flow controller Line 1 44 Mass flow controller Line 2 45 Mass flow controller Line 3 46 Mass flow controller Line 4 47 Mass flow controller Line 5 T.sub.1 Source temperature T.sub.2 Line temperature T.sub.3 Mixer temperature T.sub.4 Line temperature T.sub.5 Gas inlet temperature T.sub.6 Deposition temperature