US20050252449A1 - Control of gas flow and delivery to suppress the formation of particles in an MOCVD/ALD system - Google Patents
Control of gas flow and delivery to suppress the formation of particles in an MOCVD/ALD system Download PDFInfo
- Publication number
- US20050252449A1 US20050252449A1 US11/119,388 US11938805A US2005252449A1 US 20050252449 A1 US20050252449 A1 US 20050252449A1 US 11938805 A US11938805 A US 11938805A US 2005252449 A1 US2005252449 A1 US 2005252449A1
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- United States
- Prior art keywords
- gas
- diameter
- reservoir
- expanding channel
- process chamber
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45582—Expansion of gas before it reaches the substrate
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T50/00—Aeronautics or air transport
- Y02T50/60—Efficient propulsion technologies, e.g. for aircraft
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T137/00—Fluid handling
- Y10T137/0318—Processes
- Y10T137/0324—With control of flow by a condition or characteristic of a fluid
- Y10T137/0357—For producing uniform flow
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T137/00—Fluid handling
- Y10T137/0318—Processes
- Y10T137/0396—Involving pressure control
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T137/00—Fluid handling
- Y10T137/206—Flow affected by fluid contact, energy field or coanda effect [e.g., pure fluid device or system]
- Y10T137/2087—Means to cause rotational flow of fluid [e.g., vortex generator]
Definitions
- Embodiments of the present invention generally relate to an apparatus and a method to deposit materials on substrates, and more specifically, to an apparatus and a method for depositing hafnium-containing compounds, such as hafnium oxides or hafnium silicates using atomic layer deposition processes.
- hafnium-containing compounds such as hafnium oxides or hafnium silicates using atomic layer deposition processes.
- ALD atomic layer deposition
- reactants are sequentially introduced into a processing chamber where each reactant chemisorbs onto the substrate surface and a reaction occurs.
- a purge step is typically carried out between the deliveries of each reactant gas.
- the purge step may be a continuous purge with the carrier gas or a pulse purge between the deliveries of the reactant gases.
- Controlled and repeatable reactive gas delivery and particle suppression are challenges for advanced ALD processing to deposit films, especially for depositing hafnium-containing compounds. Therefore, there is a need for an ALD apparatus to deposit materials, such as hafnium oxides and hafnium silicates, that are repeatable and under control with adequate particle suppression.
- the embodiments of the invention describe a process chamber that has gas conduits with gradually increasing diameters to reduce Joule-Thompson effect during gas delivery, a gas liner leveled with the substrate support to sustain gas temperature and to reduce gas flow to the substrate support backside, and a gas reservoir to allow controlled delivery of process gas.
- a gas delivery assembly comprises a covering member comprising an expanding channel at a central portion of the covering member which comprises a bottom surface extending from the expanding channel to a peripheral portion of the covering member, and at least one gas conduit having a first end, with a first diameter, connected to a gas inlet of the expanding channel, and a second end, with a second diameter, connected to a valve, wherein the second diameter is greater than the first diameter and the diameter of the at least one gas conduit gradually and continuously increases from the second diameter to the first diameter, and the at least one gas conduit is positioned at an angle from a center of the expanding channel.
- an ALD process chamber comprises a ring-shaped gas liner placed between the substrate support and between the chamber wall, wherein the top surface of the ring-shaped liner is at the same level as the substrate support during exhaust gas being pumped out the process chamber.
- an ALD process chamber comprises at least one reservoir to store one process gas, wherein the first end of the at least one reservoir is coupled to a gas valve that connects to a gas conduit with a length between about 3 cm to about 10 cm connecting a gas inlet of the process chamber and the second end of the at least one reservoir couples to a gas source, and the diameter of the first end of the at least one reservoir gradually and continuously reduces to the diameter of an inlet of the gas valve and the diameter of the second end of the at least one reservoir gradually and continuously reduces to a diameter of a gas line that connects with the gas source.
- an ALD process chamber comprises a covering member comprising an expanding channel at a central portion of the covering member which comprises a bottom surface extending from the expanding channel to a peripheral portion of the covering member, at least one gas conduit having a first end, with a first diameter, connected to a gas inlet of the expanding channel, and a second end, with a second diameter, connected to a gas valve, wherein the second diameter is greater than the first diameter and the diameter of the at least one gas conduit gradually and continuously increases from the second diameter to the first diameter, and the at least one gas conduit is positioned at an angle from a center of the expanding channel, and at least one reservoir to store one process gas, wherein the first end of the at least one reservoir is coupled to the gas valve that connects to the at least one gas conduit and the second end of the at least one reservoir couples to a gas source, and the diameter of the first end of the at least one reservoir gradually and continuously reduces to a third diameter of an inlet of the gas valve and the diameter of the second end of the at least one reservoir gradually and
- a method of delivering gases to a substrate in a substrate processing chamber comprises providing at least one gas into the substrate processing chamber from a reservoir wherein the first end of the reservoir is coupled to a gas valve that connects to a gas conduit, wherein the gas conduit having a first end, with a first diameter, connected to a gas inlet of a expanding channel of the substrate processing chamber, and a second end, with a second diameter, connected to the gas valve, wherein the second diameter is greater than the first diameter and the diameter of the gas conduit gradually and continuously increases from the second diameter to the first diameter, and the gas conduit is positioned at an angle from a center of the expanding channel, and the second end of the reservoir couples to a gas source, and the diameter of the first end of the reservoir gradually and continuously reduces to a third diameter of an inlet of the gas valve and the diameter of the second end of the reservoir gradually and continuously reduces to a fourth diameter of a gas line that connects with the gas source, and providing the gases to a central portion of the substrate.
- FIG. 1 depicts a schematic cross-sectional view of one embodiment of an ALD process chamber of the current invention.
- FIG. 2A shows the simulation result of gas temperature along a conventional gas conduit.
- FIG. 2B shows the vapor pressures of hafnium precursors as a function of temperature.
- FIG. 3A depicts a schematic drawing of one embodiment of gas conduits of current invention for delivering process gas(es) into the process chamber.
- FIG. 3B shows examples of various profiles of gas conduits of the current invention.
- FIG. 3C shows the simulation result of gas temperature along one embodiment of a gas conduit of the current invention.
- FIG. 4B depicts a schematic cross-sectional view of the expanding channel of the chamber lid of FIG. 1 .
- FIG. 5A illustrates a schematic view of the process chamber with a liner between the substrate support and the chamber sidewall.
- FIG. 5B shows the simulation results of temperature along line “L” in the process chamber of FIG. 6 with and without the liner.
- FIG. 5C shows the flow dynamic simulation of gas flow of process exhaust gas and purge gas in the process chamber.
- FIG. 6A depicts a schematic drawing of two examples of gas reservoirs of the current invention.
- FIG. 6B depicts a schematic drawing of exemplary gas reservoirs connected to the expanding gas conduits of the current invention.
- FIG. 7 illustrates a process sequence for a hafnium-containing compound using an ALD technique.
- the present invention describes embodiments of an apparatus and a method for depositing a thin film by processes such as atomic layer deposition. More specifically, the present invention describes embodiment of an ALD apparatus for preparing hafnium-containing compounds used in a variety of applications, including high-k dielectric materials.
- ALD atomic layer deposition
- cyclical deposition refers to the sequential introduction of two or more reactive compounds to deposit a layer of material on a substrate surface.
- the two, three or more reactive compounds may alternatively be introduced into a reaction zone of a processing chamber.
- each reactive compound is separated by a time delay to allow each compound to adhere and/or react on the substrate surface.
- a first precursor or compound A such as a hafnium precursor
- a second precursor or compound B such as an oxidizing gas
- the oxidizing gas may include several oxidizing agent, such as in-situ water and oxygen.
- a purge gas such as nitrogen
- the purge gas may flow continuously throughout the deposition process so that only the purge gas flows during the time delay between pulses of reactive compounds.
- the reactive compounds are alternatively pulsed until a desired film or film thickness is formed on the substrate surface.
- the ALD process of pulsing compound A, purge gas, pulsing compound B and purge gas is a cycle.
- a cycle can start with either compound A or compound B and continue the respective order of the cycle until achieving a film with the desired thickness.
- FIG. 1 is a schematic cross-sectional view of an exemplary process chamber 680 including a gas delivery apparatus 730 adapted for cyclic deposition, such as atomic layer deposition or rapid chemical vapor deposition.
- a gas delivery apparatus 730 adapted for cyclic deposition, such as atomic layer deposition or rapid chemical vapor deposition.
- the terms atomic layer deposition (ALD) and rapid chemical vapor deposition as used herein refer to the sequential introduction of reactants to deposit a thin layer over a substrate structure. The sequential introduction of reactants may be repeated to deposit a plurality of thin layers to form a conformal layer to a desired thickness.
- the process chamber 680 may also be adapted for other deposition techniques.
- the process chamber 680 comprises a chamber body 682 having sidewalls 684 and a bottom 686 .
- a slit valve 688 in the process chamber 680 provides access for a robot (not shown) to deliver and retrieve a substrate 690 , such as a semiconductor wafer with a diameter of 200 mm or 300 mm or a glass substrate, from the process chamber 680 .
- the process chamber 680 could be various types of ALD chambers.
- the details of exemplary process chamber 680 are described in commonly assigned U.S. Patent Application Publication Nu. 60/570,173, filed on May 12, 2004, entitled “Atomic Layer Deposition of Hafnium-containing High-k Materials, U.S. Patent Application Publication No. 20030079686, filed on Dec. 21, 2001, entitled “Gas Delivery Apparatus and Method For Atomic Layer Deposition”, which are both incorporated herein in their entirety by references.
- a substrate support 692 supports the substrate 690 on a substrate receiving surface 691 in the process chamber 680 .
- the substrate support (or pedestal) 692 is mounted to a lift motor 714 to raise and lower the substrate support 692 and a substrate 90 disposed thereon.
- a lift plate 716 connected to a lift motor 718 is mounted in the process chamber 680 and raises and lowers pins 720 movably disposed through the substrate support 692 .
- the pins 720 raise and lower the substrate 690 over the surface of the substrate support 692 .
- the substrate support 692 may include a vacuum chuck, an electrostatic chuck, or a clamp ring for securing the substrate 690 to the substrate support 692 during processing.
- the substrate support 692 may be heated to increase the temperature of a substrate 690 disposed thereon.
- the substrate support 692 may be heated using an embedded heating element, such as a resistive heater, or may be heated using radiant heat, such as heating lamps disposed above the substrate support 692 .
- a purge ring 722 may be disposed on the substrate support 692 to define a purge channel 724 which provides a purge gas to a peripheral portion of the substrate 690 to prevent deposition thereon.
- a gas delivery apparatus 730 is disposed at an upper portion of the chamber body 682 to provide a gas, such as a process gas and/or a purge gas, to the process chamber 680 .
- a vacuum system 778 is in communication with a pumping channel 779 to evacuate any desired gases from the process chamber 680 and to help maintain a desired pressure or a desired pressure range inside a pumping zone 766 of the process chamber 680 .
- the chamber depicted by FIG. 1 permits the process gas and/or purge gas to enter the process chamber 680 normal (i.e., 90°) with respect to the plane of the substrate 690 via the gas delivery apparatus 730 . Therefore, the surface of substrate 690 is symmetrically exposed to gases that allow uniform film formation on substrates.
- the process gas may include a hafnium-containing compound (e.g., TDEAH or HfCl 4 ) during one pulse and includes an oxidizing gas (e.g., water vapor) in another pulse.
- Process chamber 680 may dose a hafnium-containing compound for about 20 seconds or less, preferably process chamber 680 may dose the hafnium-containing compound for about 10 seconds or less, more preferably for about 5 second or less.
- the process chamber 680 may be adapted to receive three or four gas flows through three or four gas inlets from three gas conduits. Each conduit is coupled to a single or plurality of valves. Further disclosure of process chamber 680 adapted to flow three process gas flows is described in paragraph 66 of commonly assigned U.S. Patent Application Publication No. 20030079686, which is both incorporated herein by reference.
- the three gas flows may be a hafnium precursor, a silicon precursor and an oxidizing gas, for example, the first flow includes HfCl 4 , the second flow includes (Me 2 N) 3 SiH and the third flow includes water vapor from a WVG system.
- the gas delivery apparatus 730 comprises a chamber lid 732 .
- the chamber lid 732 includes an expanding channel 734 extending from a central portion of the chamber lid 732 and a bottom surface 760 extending from the expanding channel 734 to a peripheral portion of the chamber lid 732 .
- the bottom surface 760 is sized and shaped to substantially cover a substrate 690 disposed on the substrate support 692 .
- the chamber lid 732 may have a choke 762 at a peripheral portion of the chamber lid 732 adjacent the periphery of the substrate 690 .
- the cap portion 772 includes a portion of the expanding channel 734 and gas inlets 736 A, 736 B, 736 C, 736 D.
- the expanding channel 734 has gas inlets 736 A, 736 B, 736 C, 736 D to provide gas flows from two similar valves 742 A, 742 B, 742 C, 742 D.
- the gas flows from the valves 742 A, 742 B, 742 C, 742 D may be provided together and/or separately.
- valves 742 A, 742 B, 742 C, and 742 D are coupled to separate reactant gas sources but are preferably coupled to the same purge gas source.
- valve 742 A is coupled to reactant gas source 738 A and valve 742 B is coupled to reactant gas source 738 B, and both valves 742 A, 742 B are coupled to purge gas source 740 .
- Each valve 742 A, 742 B, 742 C, 742 D includes a delivery line 743 A, 743 B, 743 C 743 D.
- the delivery line 743 A, 743 B, 743 C, 743 D is in communication with the reactant gas source 738 A, 738 B, 738 C, 738 D and is in communication with the gas inlet 736 A, 736 B, 736 C, 736 D of the expanding channel 734 through gas conduits 750 A, 750 B, 750 C, 750 D.
- Additional reactant gas sources, delivery lines, gas inlets and valves may be added to the gas delivery apparatus 730 in one embodiment (not shown).
- the purge lines, 745 A, 745 B, 745 C, and 745 D are in communication with the purge gas source 740 , and the flows of the purge lines, 745 A, 745 B, 745 C, and 745 D, are controlled by valves, 746 A, 746 B, 746 C, and 746 D, respectively.
- the purge lines, 745 A, 745 B, 745 C, and 745 D intersect the delivery line 743 A, 743 B, 743 C, 743 D at the valves, 742 A, 742 B, 742 C, and 742 D.
- a carrier gas is used to deliver reactant gases from the reactant gas source 738 A, 738 B, 738 C, 738 D
- a purge gas e.g., nitrogen used as a carrier gas and a purge gas.
- the valves, 742 A, 742 B, 742 C, and 742 D comprise diaphragms.
- the diaphragms may be biased open or closed and may be actuated closed or open respectively.
- the diaphragms may be pneumatically actuated or may be electrically actuated. Examples of pneumatically actuated valves include pneumatically actuated valves available from Swagelock of Solon, Ohio.
- Pneumatically actuated valves may provide pulses of gases in time periods as low as about 0.020 second.
- Electrically actuated valves may provide pulses of gases in time periods as low as about 0.005 second.
- An electrically actuated valve typically requires the use of a driver coupled between the valve and the programmable logic controller, such as 748 A, 748 B.
- Each valve 742 A, 742 B, 742 C, 742 D may be adapted to provide a combined gas flow and/or separate gas flows of the reactant gas 738 A, 738 B, 738 C, 738 D and the purge gas 740 .
- a combined gas flow of the reactant gas 738 A and the purge gas 740 provided by valve 742 A comprises a continuous flow of a purge gas from the purge gas source 740 through purge line 745 A and pulses of a reactant gas from the reactant gas source 738 A through delivery line 743 A.
- the delivery lines, 743 A, 743 B, 743 C, and 743 D of the valves, 742 A, 742 B, 742 C, and 742 D may be coupled to the gas inlets, 736 A, 736 B, 736 C, and 736 D, through gas conduits, 750 A, 750 B, 750 C, and 750 D.
- the gas conduits, 750 A, 750 B, 750 C, and 750 D may be integrated or may be separate from the valves, 742 A, 742 B, 742 C, and 742 D.
- valves 742 A, 742 B, 742 C, 742 D are coupled in close proximity to the expanding channel 734 to reduce any unnecessary volume of the delivery line 743 A, 743 B, 743 C, 743 D and the gas conduits 750 A, 750 B, 750 C, 750 D between the valves 742 A, 742 B, 742 C, 742 D and the gas inlets 736 A, 736 B, 736 C, 736 D.
- the gas inlets 736 A, 736 B, 736 C, 736 D are located adjacent the upper portion 737 of the expanding channel 734 . In other embodiments, one or more gas inlets may be located along the length of the expanding channel 734 between the upper portion 737 and the lower portion 735 .
- the hafnium precursor such as HfCl 4
- a precursor bubbler at a temperature from about 150° C. to about 200° C. and is carried into the one of the gas inlets, such as 736 A or 736 B.
- the hafnium precursor is introduced through the gas line into the process chamber 734 , due to the pressure within the delivery line is considerably higher than the pressure in the process chamber, the gas delivered to the process chamber expand rapidly and the temperature of the gases drops. This is the “Joule-Thompson effect”. This is also true when the water vapor is introduced into the process chamber.
- this temperature drop can have unwanted consequences. For example, consider the case of a gas delivering a low vapor pressure reactant. If this gas undergoes rapid expansion (the accompanying rapid cooling) as it leaves the manifold and enters the process chamber, the reactant may condense from vapor phase and precipitate into fine particles. Similarly, when the temperature drops below 100° C., water vapor also condenses into liquid.
- FIG. 2A shows the simulated temperature drop of N 2 gas along an about 5 cm gas conduit with constant diameter.
- CFD-ACE+ is a general, partial differential equation (PDE) solver for a broad range of physics disciplines including: flow, heat transfer, stress/deformation, chemical kinetics, electrochemistry, and others. It solves them in multidimensional (0D to 3D), steady and transient form.
- PDE partial differential equation
- CFD-ACE+ is used for complex multi-physics and multidisciplinary applications.
- the temperature drops from 200° C. to 108° C.
- FIG. 2B shows the vapor pressure of several hafnium precursors as function of temperature.
- a gradually and continuously expanding gas conduit is believed to reduce the Joule-Thompson effect of gas expansion.
- the disclosed gas conduit design prevents large temperature drops by allowing the gases to expand gradually and continuously. This is accomplished by gradually and continuously increasing or tapering the flow channel cross-section.
- the flow channel transitions from the cross-sections of delivery gas lines with internal diameter of between about 3 mm to about 15 mm to a larger chamber inlet with diameter between about 10 mm to about 20 mm over a distance between about 30 mm to about 100 mm.
- the gradually and continuously expanding channel may comprise one or more tapered inner surfaces (shown in FIG. 3B ), such as a tapered straight surface, a concave surface, a convex surface, or combinations thereof or may comprise sections of one or more tapered inner surfaces (i.e., a portion tapered and a portion non-tapered).
- the shapes and sizes of the gas conduits, such as 750 A, 750 B, 750 C, and 750 D, do not have to be the same for a process chamber.
- FIG. 3C shows simulated results of the temperature drop along the about 5 cm tapered gas conduits, 750 A, 750 B, 750 C, and 750 D, of FIGS. 1 and 3 A.
- the temperature drops only slightly from 190° C. to 183° C., in contrast to large temperature drop of 200° C. to 108° C. of the conventional design as shown in FIG. 4 .
- Gas conduit temperature maintaining above 180° C. helps to keep the hafnium precursor in vapor form. As evidenced by computer simulations data, the gas flow in the gas conduit design with tapered flow channels experiences a smaller temperature drop.
- FIG. 4A is a top cross-sectional view of one embodiment of the expanding section 734 of the chamber lid 732 of FIG. 1 .
- Each gas conduit such as 750 A, 750 B, may be positioned at an angle ⁇ from the center line 702 of the gas conduit, such as 750 A, 750 B, and from a radius line 704 from the center of the expanding channel 734 .
- Entry of a gas through the gas conduit 750 A, 750 B preferably positioned at an angle ⁇ (i.e., when ⁇ >0°) causes the gas to flow in a circular direction as shown by arrow 710 A (or 710 B).
- Providing gas at an angle ⁇ as opposed to directly straight-on to the walls of the expanding channel i.e.
- gas conduits such as 750 A, 750 B, and the corresponding gas inlets 736 A, 736 B are spaced out from each other and direct a flow in the same circular direction (i.e., clockwise or counter-clockwise).
- Gas conduits, 750 C and 750 D can be placed below gas conduits, 750 A and 750 B, respectively along the expanding channel 734 , or be placed next to gas conduits 750 A, 750 B and be on the plane level as the gas conduits 750 A, 750 B.
- FIG. 4B is a cross-sectional view of the expanding channel 734 of a chamber lid 732 showing simplified representations of two gas flows therethrough.
- the circular flow 710 may travel as a “vortex,” “helix,” or “spiral” flow 902 A, 902 B through the expanding channel 734 as shown by arrows 902 A, 902 B.
- the circular flow may be provided in a “processing region” as opposed to in a compartment separated from the substrate 690 .
- the vortex flow may help to establish a more efficient purge of the expanding channel 734 due to the sweeping action of the vortex flow pattern across the inner surface of the expanding channel 734 .
- the distance 710 A between the gas inlets 736 A, 736 B and the substrate 690 is made far enough that the “vortex” flow 902 dissipates to a downwardly flow as shown by arrows 904 as a spiral flow across the surface of the substrate 690 may not be desirable. It is believed that the “vortex” flow 902 and the downwardly flow 904 proceeds in a laminar manner efficiently purging the chamber lid 732 and the substrate 690 .
- the distance 710 A, 710 B between the upper portion 737 of the expanding channel 734 and the substrate 690 is about 1.0 inches or more, more preferably about 2.0 inches or more. In one specific embodiment, the upper limit of the distance 710 A, 710 B is dictated by practical limitations.
- the upper limit of distance 710 A, 710 B may be 3 inches or more for a chamber adapted to process 200 mm diameter substrates or 5 inches or more for a chamber adapted to process 300 mm diameter substrates.
- the bottom surface 760 of the chamber lid 732 may be tapered from the expanding channel 734 to a peripheral portion of the chamber lid 732 to help provide an improved velocity profile of a gas flow from the expanding channel 734 across the surface of the substrate 690 (i.e., from the center of the substrate to the edge of the substrate).
- the bottom surface 760 may comprise one or more tapered surfaces, such as a straight surface, a concave surface, a convex surface, or combinations thereof.
- the bottom surface 760 is tapered in the shape of a funnel.
- FIG. 5A shows a schematic drawing of an ALD chamber with a gas liner 888 .
- the gas liner 888 is close to the pedestal 692 to take more heat from the pedestal. This would keep the gas liner 888 at elevated temperature, preferably above 100° C., to prevent water vapor from condensing into liquid form at the liner.
- the liner is leveled with the substrate support during process exhaust gas being pumped out and also fill most of the space between the substrate support 692 and the chamber sidewall 684 ; therefore, the gas liner 888 prevents the process exhaust gas from escaping to the region below the substrate support 692 and prevents process exhaust gas from create back side deposition on the pedestal 692 .
- the liner 888 is ring-shaped and it fits between the substrate support and the chamber wall.
- the liner's inside wall 887 should be very close to the pedestal 692 to take heat from the pedestal heater via convention, conduction and radiation heat transfer. This would make the temperature of the liner to be at desired temperature of about 100° C.
- the distance between the liner's inside wall 887 to the pedestal (or substrate support) 692 is between about 0.1 inch (or 0.25 cm) to about 0.5 inch (or 1.27 cm). When the liner 888 is at this elevated temperature of about 100° C., the water vapor will not condense on the liner's wall.
- the liner's outside wall 886 should also be very close to the chamber inner wall 684 to prevent process exhaust gas from escaping to the backside of the pedestal 692 (or 812 ).
- the distance between the liner's outside wall 886 to the chamber inner wall 684 is between about 0.1 inch (or 0.25 cm) to about 0.5 inch (or 1.27 cm).
- FIG. 8 shows the temperature simulation results of along line “L” of reactors between the substrate support 692 and the part of chamber wall 684 of FIG. 5A .
- Curve 801 shows the simulated temperature with the liner 888
- curve 802 shows the simulated temperature without the liner 888 .
- the temperature of chamber wall 684 is about 85° C. with or without liner. However, liner maintains the temperature at above 105° C., until it reaches the chamber wall 684 . This helps to keep the water vapor in gas form.
- FIG. 5B shows a flow modeling on the design to predict the effectiveness of the design. The flow simulation that gas(es) would be pumped out before reaching the back of the pedestal heater.
- CFD-ACE+ computation fluid dynamics software is used to perform the flow simulation.
- the materials for the liner 888 depends on the nature of the process gases.
- the liner 888 can be made of materials such as aluminum, if the process gas is non-corrosive, such as TDEAH.
- the liner 888 can also be made of corrosion-resistant materials, such as quartz or pyrolitic boron nitride, if the process gas is corrosive, such as HfCl 4 .
- the existing design of the gas delivery has limitation on how much reactive precursor can be delivered to the process chamber in a short amount of time.
- Advanced ALD process requires the precursor to be delivered to the process chamber in a short time, such as between about 50 ms to about 3 seconds to ensure high substrate processing throughput, and under stable and repeatable temperature to minimize temperature fluctuation and to ensure low particle counts.
- the gas valve such as 742 A, 742 B, 742 C and 742 D
- the process gas would burst into the process chamber and cause the gas pressure in the gas conduit, such as 750 A, 750 B, 750 C, and 750 D, to drop quickly.
- the gas conduit such as 750 A, 750 B, 750 C, and 750 D
- the precise control of pressure in the gas conduit(s) and amount of process gas delivered is very important. Since the pulsing of the process gas, such as hafnium precursor gas, could only take 2 seconds or below, the time it take to recover pressure in the gas conduit makes the precise control of advanced ALD processing impossible.
- FIG. 6A shows the two exemplary designs (A and B) of a reservoir 889 B, which is coupled to the valves 742 B and gas source 738 B.
- the reservoir 889 has a large volume between about 80 cc to about 200 cc to store reactive precursor gas, which could be introduced at a higher amount during process.
- the gas reservoir 889 is also designed to have gradual increased diameters at two ends to reduce the Joule-Thompson effect mentioned above. The gradual increased diameters at the two ends of the reservoir allows for even temperature distribution across the reservoir at all time.
- the reservoir 889 B was designed to allow for a higher volume of the precursor closer to the point of use.
- the outlet of the gas reservoir 889 B, or the end that is connected a valve 742 B that couples to a gas conduit 750 B (not shown here) to the process chamber, should be at the same level as the gas conduit 750 B to avoid needing to bend the gas line. Bending the gas line at an angle, such as 90 degree, could cause the gas velocity to drop and could result in change of gas temperature.
- the gas reservoirs 889 A, 889 B, 889 C, 889 D can be coupled to one of the gas conduits 750 A, 750 B, 750 C, 750 D which is attached to gas inlets 736 A, 736 B, 736 C, 736 D to reduce the Joule-Thompson effect of gas expansion when the process gas is introduced into the expanding channel 734 , as shown in FIG. 6B .
- the reservoir is made by drilling out the desired shape out of an aluminum bulk on the lid of the chamber to allow for even thermal distribution. Heating materials can be buried in the aluminum bulk to keep the temperature of the gas reservoir constant.
- the reservoir can be made of other types of conductive materials to allow sufficient heat transfer to maintain the gas temperature.
- the reservoir can also be made of sheet of conductive material, such as aluminum sheet, and be wrapped with heating medium to control temperature in the reservoir.
- a control unit 780 such as a programmed personal computer, work station computer, or the like, may be coupled to the process chamber 680 to control processing conditions.
- the control unit 780 may be configured to control flow of various process gases and purge gases from gas sources 738 A, 738 B, 738 C, 738 D, 740 through the valves 742 A, 742 B, 742 C, 742 D, 746 A, 746 B, 746 C, 746 D during different stages of a substrate process sequence.
- the control unit 780 comprises a central processing unit (CPU) 782 , support circuitry 784 , and memory 786 containing associated control software 783 .
- CPU central processing unit
- FIG. 7 illustrates an exemplary process sequence 100 for forming a hafnium-containing material, such as hafnium oxide, according to one embodiment of the present invention.
- a substrate to be processed is first loaded into a process chamber capable of performing cyclical deposition and the process conditions are adjusted (step 110 ).
- Process conditions may include temperature, pressure and flow rate of carrier gas.
- the substrate is then exposed to pulse of a hafnium precursor that is introduced into the process chamber for a time period in a range from about 0.1 second to about 5 seconds (step 120 ).
- a pulse of purge gas is then pulsed into the processing chamber (step 130 ) to purge or otherwise remove any residual hafnium precursor or by-products.
- a pulse of oxidizing gas is introduced into the processing chamber (step 140 ).
- the oxidizing gas may include several oxidizing agents, such as in-situ water and oxygen.
- a pulse of purge gas is then introduced into the processing chamber (step 150 ) to purge or otherwise remove any residual oxidizing gas or by-products.
- Suitable carrier gases or purge gases may include helium, argon, nitrogen, hydrogen, forming gas, oxygen and combinations thereof.
- a “pulse” as used herein is intended to refer to a quantity of a particular compound that is intermittently or non-continuously introduced into a reaction zone of a processing chamber.
- a hafnium-containing compound such as hafnium oxide, having a particular thickness will be deposited on the substrate surface.
- each deposition cycle forms a layer with a thickness in the range from about 1 ⁇ to about 10 ⁇ .
- subsequent deposition cycles may be needed to deposit hafnium-containing compound having a desired thickness.
- a deposition cycle (steps 120 through 150 ) can be repeated until the desired thickness for the hafnium-containing compound is achieved. Thereafter, the process is stopped as indicated by step 170 when the desired thickness is achieved.
- Hafnium oxide deposited by an ALD process has the empirical chemical formula HfO x .
- Hafnium oxide has the molecular chemical formula HfO 2 , but by varying process conditions (e.g., timing, temperature, precursors), hafnium oxide may not be fully oxidized, such as HfO 1.8 .
- hafnium oxide is deposited by the processes herein with the molecular chemical formula of about HfO 2 or less.
- the cyclical deposition process or ALD process of FIG. 1 typically occurs at a pressure in the range from about 1 Torr to about 100 Torr, preferably in the range from about 1 Torr to about 20 Torr, for example from about 1 Torr to about 10 Torr.
- the temperature of the substrate is usually in the range from about 70° C. to about 1,000° C., preferably from about 100° C. to about 650° C., more preferably from about 250° C. to about 500° C.
- the hafnium precursor is introduced to the process chamber at a rate in the range from about 5 mg/m to about 200 mg/m.
- the hafnium precursor is usually introduced with a carrier gas, such as nitrogen, with a total flow rate in the range from about 50 sccm to about 2,000 sccm.
- a carrier gas such as nitrogen
- the hafnium precursor is pulsed into the process chamber at a duration from about 1 second to about 10 seconds, depending on the particular process and desired hafnium-containing compound.
- advanced ALD processes the hafnium precursor is pulsed into the process chamber at a shorter duration from about 50 ms to about 3 seconds.
- the hafnium precursor is generally dispensed to the process chamber 180 by introducing carrier gas into a bubbler containing the hafnium precursor.
- Suitable bubblers such as PROE-VAPTM, are available from Advanced Technology Materials, Inc., locate in Danbury, Conn.
- the temperature of the bubbler 182 is maintained at a temperature depending on the hafnium precursor within, such as from about 100° C. to about 300° C.
- the bubbler may contain HfCl 4 at a temperature from about 150° C. to about 200° C.
- the oxidizing gas is introduced to the process chamber 180 at a rate in the range from about 10 sccm to about 1,000 sccm, preferably in the range from about 30 sccm to about 200 sccm.
- the oxidizing gas is pulsed into the process chamber 180 at a rate from about 0.1 second to about 10 seconds, depending on the particular process and desired hafnium-containing compound.
- the oxidizing gas is pulsed into the process chamber at a shorter duration from about 50 ms to about 3 seconds.
- the oxidizing gas is produced from a water vapor generating (WVG) system 186 that is in fluid communication to the process chamber 180 by a line 187 .
- the WVG system 186 generates ultra-high purity water vapor by means of a catalytic reaction of O 2 and H 2 .
- the WVG system has a catalyst-lined reactor or a catalyst cartridge in which water vapor is generated by means of a chemical reaction, unlike pyrogenic generators that produce water vapor as a result of ignition. Regulating the flow of H 2 and O 2 allows the concentration to be precisely controlled at any point from 1% to 100% concentrations.
- the water vapor may contain water, H 2 , O 2 and combinations thereof.
- Suitable WVG systems are commercially available, such as the WVG by Fujikin of America, Inc., located in Santa Clara, Calif. and the CSGS (Catalyst Steam Generator System) by Ultra Clean Technology, located in Menlo Park, Calif.
- Precursors at ambient temperature and pressure may be plasma, gas, liquid or solid. However, within the ALD chamber, volatilized precursors are utilized.
- Organometallic compounds or complexes include any chemical containing a metal and at least one organic group, such as amides, alkyls, alkoxyls, alkylamidos and anilides. Precursors comprise of organometallic, inorganic and halide compounds.
- the ALD processes disclosed above may be altered by substituting the hafnium and/or silicon precursors with other metal precursors to form materials, such as hafnium aluminates, titanium silicates, zirconium oxides, zirconium silicates, zirconium aluminates, tantalum oxides, tantalum silicates, titanium oxides, titanium silicates, silicon oxides, aluminum oxides, aluminum silicates, lanthanum oxides, lanthanum silicates, lanthanum aluminates, nitrides thereof and combinations thereof.
- hafnium aluminates titanium silicates, zirconium oxides, zirconium silicates, zirconium aluminates, tantalum oxides, tantalum silicates, titanium oxides, titanium silicates, silicon oxides, aluminum oxides, aluminum silicates, lanthanum oxides, lanthanum silicates, lanthanum aluminates, nitrides thereof and combinations thereof.
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US11/925,684 US7794544B2 (en) | 2004-05-12 | 2007-10-26 | Control of gas flow and delivery to suppress the formation of particles in an MOCVD/ALD system |
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US11/127,767 Abandoned US20050271813A1 (en) | 2004-05-12 | 2005-05-12 | Apparatuses and methods for atomic layer deposition of hafnium-containing high-k dielectric materials |
US11/925,684 Expired - Fee Related US7794544B2 (en) | 2004-05-12 | 2007-10-26 | Control of gas flow and delivery to suppress the formation of particles in an MOCVD/ALD system |
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US11/925,684 Expired - Fee Related US7794544B2 (en) | 2004-05-12 | 2007-10-26 | Control of gas flow and delivery to suppress the formation of particles in an MOCVD/ALD system |
US11/925,681 Expired - Fee Related US8282992B2 (en) | 2004-05-12 | 2007-10-26 | Methods for atomic layer deposition of hafnium-containing high-K dielectric materials |
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USD990441S1 (en) | 2021-09-07 | 2023-06-27 | Asm Ip Holding B.V. | Gas flow control plate |
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Also Published As
Publication number | Publication date |
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WO2005113855A1 (en) | 2005-12-01 |
CN101052745B (zh) | 2011-02-23 |
KR101316056B1 (ko) | 2013-10-10 |
US8343279B2 (en) | 2013-01-01 |
JP2007537360A (ja) | 2007-12-20 |
US7794544B2 (en) | 2010-09-14 |
WO2005113852A3 (en) | 2006-05-18 |
US20050271813A1 (en) | 2005-12-08 |
CN1934287B (zh) | 2012-06-20 |
CN1934287A (zh) | 2007-03-21 |
JP5063344B2 (ja) | 2012-10-31 |
EP1745159A2 (en) | 2007-01-24 |
JP2007537605A (ja) | 2007-12-20 |
US20080044569A1 (en) | 2008-02-21 |
US8282992B2 (en) | 2012-10-09 |
KR20070015959A (ko) | 2007-02-06 |
CN101052745A (zh) | 2007-10-10 |
EP1745160A1 (en) | 2007-01-24 |
JP5053079B2 (ja) | 2012-10-17 |
US20050271812A1 (en) | 2005-12-08 |
WO2005113852A2 (en) | 2005-12-01 |
US20080041307A1 (en) | 2008-02-21 |
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