WO2000079019A1 - Dispositif de depot chimique en couches atomiques en phase vapeur - Google Patents

Dispositif de depot chimique en couches atomiques en phase vapeur Download PDF

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Publication number
WO2000079019A1
WO2000079019A1 PCT/US2000/017202 US0017202W WO0079019A1 WO 2000079019 A1 WO2000079019 A1 WO 2000079019A1 US 0017202 W US0017202 W US 0017202W WO 0079019 A1 WO0079019 A1 WO 0079019A1
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Prior art keywords
substrate
gas
injection tube
tube
injector
Prior art date
Application number
PCT/US2000/017202
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English (en)
Inventor
Prasad Narhar Gadgil
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Prasad Narhar Gadgil
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Publication date
Application filed by Prasad Narhar Gadgil filed Critical Prasad Narhar Gadgil
Priority to EP00950239A priority Critical patent/EP1226286A4/fr
Priority to JP2001505362A priority patent/JP2003502878A/ja
Priority to US10/019,244 priority patent/US6812157B1/en
Priority to AU63367/00A priority patent/AU6336700A/en
Publication of WO2000079019A1 publication Critical patent/WO2000079019A1/fr
Priority to US10/865,111 priority patent/US20040224504A1/en

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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
    • C23C16/458—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 supporting substrates in the reaction chamber
    • C23C16/4582—Rigid and flat substrates, e.g. plates or discs
    • C23C16/4583—Rigid and flat substrates, e.g. plates or discs the substrate being supported substantially horizontally
    • C23C16/4584—Rigid and flat substrates, e.g. plates or discs the substrate being supported substantially horizontally the substrate being rotated
    • 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
    • C23C16/45519—Inert gas curtains
    • C23C16/45521—Inert gas curtains the gas, other than thermal contact gas, being introduced the rear of the substrate to flow around its periphery
    • 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
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45544—Atomic layer deposition [ALD] characterized by the apparatus
    • C23C16/45548—Atomic layer deposition [ALD] characterized by the apparatus having arrangements for gas injection at different locations of the reactor for each ALD half-reaction
    • C23C16/45551—Atomic layer deposition [ALD] characterized by the apparatus having arrangements for gas injection at different locations of the reactor for each ALD half-reaction for relative movement of the substrate and the gas injectors or half-reaction reactor compartments
    • 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
    • C23C16/45563—Gas nozzles
    • C23C16/45578—Elongated nozzles, tubes with holes
    • 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
    • C23C16/45587—Mechanical means for changing the gas flow
    • C23C16/45589—Movable means, e.g. fans

Definitions

  • the present invention relates to thin film deposition at a single atomic layer precision for manufacturing of semiconductor devices. More particularly, this invention describes a variety of apparatus configurations to enable atomic layer chemical vapor deposition of thin films of various materials on the surface substrate.
  • ICs integrated circuits
  • silicon wafer size has progressed in recent years from
  • the critical device dimension has decreased from 0.35 micron to 0.25 micron to 0.18 micron.
  • Research and development for the future device dimension devices at 0.13 and next to 0.10-micron technologies is being conducted by several leading IC manufacturers. Such steps are necessary to increase the device speed, sophistication, capability and yield.
  • These trends in the IC production technology have placed extremely stringent and divergent demands on the performance of semiconductor manufacturing equipment that deposit, pattern or etch progressively smaller device structures on the surface of a silicon wafer. This in turn translates into extremely precise control of the critical process parameters such as film thickness, morphology, and conformal step coverage over complex topography and uniformity over an increasingly large area wafer surface.
  • temperature uniformity of the deposition surface plays an extremely crucial role in affecting the rate of film deposition. This factor being rather crucial in CVD as compared to PVD.
  • the wafer temperature must be maintained at +/- 1 degree C at 500 degree C. This leads to complex and expensive heater designs and temperature control hardware and ultimately to added cost and complexity.
  • the average rate of film deposition in CVD mode can be tailored over a wide range. The rate of deposition may be as high as 1000 A/min to as low as 100 A/min.
  • yet another fundamental shortcoming of CVD being a dynamic process (and PVD also) is extremely low degree of film uniformity below a certain minimum value of thickness, typically below 200 A (Angstrom).
  • RTCVD rapid heating and cooling may lead to wafer warping, slip and undesirable film stress.
  • RTCVD is invariably susceptible to complexities arising from undesirable deposition on windows, optical properties of chamber materials, expensive and complex hardware for optics and radiation control. Also required is the chamber construction material that can withstand rapid and repeated thermal shocks under high vacuum.
  • Atomic layer chemical vapor deposition is a simple variant of CVD. It was invented in Finland in late 70's to deposit thin and uniform films of compound semiconductors, such as zinc sulfide. There are several attributes of ALD that make it an extremely attractive and highly desirable technique for its application to microelectronic industry.
  • ALD is a flux independent technique and it is based on the principle of self-limiting surface reaction. It is also relatively temperature insensitive. In a typical ALD sequence two highly reactive gases react to form a solid film and a gaseous reaction by-product is formed. It is carried out in discrete steps as follows.
  • FIG. 1 is a schematic of a conventional ALD process cycle with two inert gas pulses and two reactive gas pulses.
  • a reactive gas (A) is pulsed over the wafer 10.
  • the gas molecules saturate the wafer 10 surface by chemically reacting with it to conform to the contours of the surface. This process is called chemisorption.
  • an inert gas (P) pulse is sent over the surface that sweeps away excess number of gas molecules that are loosely attached (physiosorbed) to the surface and thus a monolayer of highly reactive species is formed on the wafer 10 surface.
  • the second reactive gas (B) is pulsed over the wafer 10 surface.
  • ALD atomic layer deposition
  • ALD reactor All such factors not only ensure tremendous simplification in the design and operation of equipment but also its scalability without much effort. With respect to process parameters, ALD offers an unprecedented level of process control. The film thickness is controlled in a digital fashion at a single atomic level, e.g. ⁇ 3 A/cycle. Also, the ALD process being surface reaction controlled offers complete and ideal step coverage over complex topography of devices all over the wafer. High and spontaneous reactivity of two precursor gases brings extreme complications to the design and operation of a CVD reactor and adversely affects the film uniformity. In an ALD process, high and spontaneous reactivity of precursors is in fact highly desirable and is exploited to its advantage. Furthermore, in an ALD sequence, the reaction is carried to completion. This ensures complete removal of undesirable reaction by-products from the film. The completion of reaction thus leads to films that are purer and contain much smaller number of defects as compared to their CVD counterparts.
  • ALD atomic layer deposition
  • FIG. 2 shows a compact ALD reactor 12 with transverse flow configuration in which the wafer 10 lies stationary within a narrow gap in the reactor and gases A, P, and B are pulsed in from one side of the reactor. This type of reactor design has some inherent and serious drawbacks.
  • ALD is basically a slower process.
  • such a reactor 12 configuration is inherently susceptible to adverse downstream mixing of reactive gases due to flow instabilities imposed by thermal convection.
  • the pulse width is shortened the reactive gas can be depleted downstream, leaving the trailing end of the substrate surface without any coating and thus seriously and adversely affecting the ALD process.
  • v is the gas velocity and L is path length of the gas in the ALD reactor that is closely correlated to the substrate dimension. This relationship stipulates the shortest possible path length for gas flow.
  • the gas residence time above the substrate must be as small as possible.
  • the reactive gas during the pulse must completely and uniformly cover a substrate of any suitably large dimension.
  • a conventional CVD reactor configuration is a parallel plate type.
  • the reactive gases or vapors are uniformly injected, through hundreds of small holes in a plate, that is called shower-head, perpendicularly on to a heated substrate surface that is directly opposite to it.
  • Manifold plates behind the showerhead achieve the difficult task of equally distributing reactive gas mixture to each of the hundreds of holes.
  • this invariably increases the gas path length tremendously.
  • a CVD reactor may be used to perform an ALD task in principle; however, in practice it is highly inefficient and thus unsuitable.
  • the present invention provides an atomic layer deposition (ALD) reactor that includes a substantially cylindrical chamber and a substrate mounted within the chamber.
  • the ALD reactor further includes at least one injection tube mounted within the chamber having a plurality of apertures along one side that direct gas emanating from the apertures towards the substrate. While gas is pulsed from the injection tube, either the substrate or the injection tube is continuously rotated in a longitudinal plane within the chamber to ensure complete and uniform coverage of the substrate by the gas.
  • the ALD reactor covers a wafer substrate with a gas deposition sequence comprising a first reactive gas (A), an inert gas (P), the second reactive gas (B), and the inert gas (P).
  • the wafer substrate is rotated in a horizontal plane in relation to the injection tube.
  • the wafer substrate is stationery within the chamber and the injector tube is rotated in relation to the wafer substrate.
  • the ALD reactor includes three injection tubes mounted within the chamber in parallel, the first injection tube dispenses gas (A)?, the second injection tube dispenses gas (P)?, and the third injection tube dispenses gas B.
  • the at least one injection tube may be configured in a cross injector tube configuration, a radial gas injector configuration, as stacked circumferencal O-rings, or as stacked longitudinal injectors.
  • the present invention improves the efficiency of an atomic layer chemical vapor deposition apparatus.
  • a combination of relative motion of the substrate with one of the various gas injection configurations achieves complete wafer surface coverage without gas depletion in the shortest possible time frame.
  • the gas injection configurations are highly suitable to realize large area, uniform and highly conformal atomic layer deposition with precise process control.
  • FIG. 1 shows the schematic of an ALD process cycle with two inert gas pulses and two reactive gas pulses.
  • FIG. 2 shows the compact ALD reactor with transverse flow configuration.
  • FIG. 3 shows configurations of injector tubes in an ALD reactor.
  • FIG. 4 A shows the schematic of an ALD reactor with three fixed gas injector tubes and a rotating susceptor.
  • FIG. 4B shows the details of the susceptor, heater support, rotation mechanism and purge gas assembly.
  • FIG. 5 shows the top view of the ALD reactor with RF electrodes for generating a suitable plasma.
  • FIG. 6 shows the gas pulse-rotation synchronization for a typical ALD deposition sequence, where T is the time required for one complete rotation of the substrate around its vertical axis and the Y-axis denotes quantity of the gas at an arbitrary scale.
  • FIG. 7 shows the top view of an alternative configuration of an ALD reactor with RF electrodes for generating a suitable plasma.
  • FIG. 8 shows the top view of an alternative configuration of an ALD reactor with multiple gas inlets for fabrication of atomic layers of non-stoichiometric materials.
  • FIG. 9 shows the top view of an alternative configuration of an ALD reactor multiple gas inlets for fabrication of atomic layers of non-stoichiometric materials.
  • FIG. 10 shows the schematic of cross injector tube assembly.
  • FIG. 11 shows the schematic of an ALD reactor with radial gas injector configuration.
  • FIG. 12 shows the Schematic of an ALD reactor with gas injection on a rotating substrate with stacked, peripheral O- rings.
  • FIG. 13 shows the lateral gas injection from stacked and longitudinal gas injectors on a rotating substrate.
  • FIG. 14 shows the schematic of an inverted ALD reactor with a stationary "upside-down" substrate and rotating injector tubes providing an upward flow injection.
  • the present invention relates to thin film deposition at a single atomic layer precision for manufacturing of semiconductor devices.
  • the following description is presented to enable one of ordinary skill in the art to make and use the invention and is provided in the context of a patent application and its requirements. Various modifications to the preferred embodiment will be readily apparent to those skilled in the art and the generic principles herein may be applied to other embodiments. Thus, the present invention is not intended to be limited to the embodiment shown but is to be accorded the widest scope consistent with the principles and features described herein.
  • This pressing invention provides atomic layer deposition (ALD) apparatus configurations that can achieve complete wafer substrate coverage by reactive gases in a shortest path length with flow stability and in a compact volume.
  • a combination of relative motion of the substrate with one of the various gas injection schemes in the form of projecting gas jets achieves complete surface coverage without gas depletion.
  • the operational range of process development for the atomic layer deposition configurations is sufficiently wide with respect to pressure and temperature. At high pressures, the jets are confined to the vicinity of their respective axes whereas, at low pressure they tend to expand laterally.
  • the suitable operational pressure range may be from 760 Torr to several milli-Torr.
  • the reaction temperature is dependent upon the reaction chemistry. It is highly desirable to set the flow rate in ALD at the minimum, but sufficient to obtain complete and uniform surface coverage with the help of mass flow controllers, so as to maximize the usage of reactants.
  • a compact, shortest path length atomic layer chemical vapor deposition chamber comprising a body that is substantially cylindrical in shape, such that the height is preferably less than its diameter.
  • a substrate holder is co-axially mounted so as to define an annular gap there between.
  • a substrate-processing region is adapted to enclose the substrate during processing.
  • a load unload port opening to the substrate- processing region is provided to transfer the substrate into and out of the substrate- processing region.
  • a remotely operable vacuum valve is provided to open and close the load/unload port opening. The vacuum valve is adapted to provide a vacuum, seal to the chamber in the closed position.
  • the substrate- processing region is interposed between the gas injection region and the pedestal region that supports the substrate during processing.
  • the gas injection region comprises one or more gas and vapor injection inlets, each with a suitable pneumatic valve that is normally closed and an upstream mass flow controller to measure the quantity of reactive gas and/or vapor flowing through it.
  • the gas injection inlets open into the substrate-processing region.
  • the pedestal region incorporates a heater that supplies the heat energy to the substrate to affect the desired chemical reaction and there are also cooling lines adapted to cool the body of the chamber and also the lid of the chamber that houses injector tubes.
  • the pedestal is mounted co-axially to the body of the chamber, on a device that enables the rotation of the pedestal around its vertical common axis at a constant and pre-defined angular velocity.
  • An exhaust exit is adapted suitably in the vicinity of the pedestal region for evacuating the gas and vapor from the chamber.
  • an injection tube with one end closed, or both ends closed with a center gas inlet, and with appropriately spaced flow openings along its length, is connected to the gas injection port that is connected to the gas or vapor source of a first type through a remotely operable pneumatic valve and a mass flow controller.
  • the gas injection port is attached either at the center of the tube or at one of its ends.
  • the portion of the tube with openings generally exceeds the diameter of the substrate.
  • the injection tube is placed parallel to the and in close proximity of principle diagonal of the chamber.
  • the tube faces the substrate such that the jets of gas or vapor emanating from the openings in it impinge directly on the diameter of the substrate at an angle that is preferably smaller than 90 degrees. In preferred embodiment, the value of this angle is approximately between 10 and 20 degrees with respect to the normal.
  • a second tube connected to a pneumatic valve that is connected to a mass flow controller that is connected to a gas or vapor source of second type, is spaced preferably parallel to the principle diagonal of the chamber in close proximity, but equi-distance opposite to the first tube from the principle diagonal.
  • the gas and vapor jets emanating from the openings in the wall of the second tube impinge directly on the diameter of the substrate that is co-axially mounted on a pedestal.
  • a third tube, with suitably spaced apertures along its wall, that is connected to a pneumatic valve that is connected to a mass flow controller is mounted exactly along the principle diagonal of the chamber such that the jets emanating from it directly impinge on the diameter of the substrate.
  • FIG. 3 A and 3B show configurations of injector tubes in an ALD reactor for use in a preferred embodiment of the present invention.
  • an injector tube 14A is shown having apertures along its radius R (where R matches or exceeds the radius of the substrate), a center fed inlet of gaseous reactants of concentration C, and both ends of the tube closed. Radial concentrations Cl, C2 ....Cn increase towards the edge of the substrate, and the concentration profile is symmetric with respect to the centerline.
  • 3B shows an end feed injector tube 14B having an end fed gas inlet of concentration C and the other end closed.
  • Concentrations Cn, ....C2, Cl decrease towards the centerline and again symmetrically increase towards the trailing edge of the tube 14B past the centerline, in the direction of flow.
  • the adverse effects of depletion of the reactant within the tube and simultaneous increase in the area of the sector of the substrate that is proportional to the square of the radius, must be countered appropriately. It is highly important for the efficient operation of the ALD reactor, in such a configuration, that the amount of gaseous reactant being ejected on the substrate diagonal increases proportionately as it progresses radially outward from the center in both directions within the tube. This is achieved by one or more means as follows:
  • FIG. 4A shows a schematic of an ALD reactor 13 comprising a substantially cylindrical chamber 15 having a substrate processing region with three fixed gas injector tubes 14 and a rotating susceptor 16 for holing a wafer substrate 22.
  • a and B are reactive gas supplies and P is an inert gas supply, which are provided by mass flow controllers 18. Gas jets emanating from slots in three fixed tubes 14A, 14B, and 14C impinge directly on the diagonal of a wafer substrate 22.
  • a pulse-rotation syncrhonization mechanism 24 ensures that the rotating susceptor 16 rotates the substrate 22 in a horizontal plane around its vertical axis at a constant angular velocity in a synchronized fashion with the gas pulses, which are controlled by pneumatic values 20. Synchronization may not be entirely necessary as long as the wafer completes at least l A rotation during the pulse width of the gases A, B and P.
  • FIG. 4B shows the details of susceptor 16, encapsulated heater 26 , rotation mechanism 28 and purge gas assembly.
  • the susceptor 16 is a co-axially mounted pedestal that holds the substrate 22 in a horizontal plane with the gas injector tubes 14 directly opposite to it.
  • a resistance or an infrared lamp heater 26 is mounted co-axially and directly underneath in close proximity to the susceptor 16 to heat the substrate 22 to a uniform and constant desired temperature in closed loop control mode.
  • the heater 26 is either hermetically sealed and /or is housed in an enclosure 30 that is continuously being purged by an inert gas. The inert gas pressure inside enclosure 30 is maintained higher than the chamber pressure.
  • the rotation device also hermetically sealed and/or purged, to impart a constant angular motion to the susceptor 16 is mounted co-axially and directly underneath the heater 26.
  • An inert gas flowing through the rotation device 28 and the heater cavity is subsequently bled in the gap between the susceptor 16 and heater 26 such that it flows radially outwards. Rotation of the susceptor 16 and the switching of pneumatic valves on each injector tube is precisely synchronized for maximum efficient operation of the reactor.
  • a first type of reactive gas or vapor (e.g. gas or vapor A) is injected through tube 14A by opening the pneumatic valve such that the gas or vapor jets strike the diagonal of the substrate 22.
  • Synchronization mechanism ensures that the substrate 22 rotates through 180 degrees or one half of the complete rotation during which time period the first type of reactive gas or vapor is injected directly on the diagonal of the substrate 22.
  • the pneumatic valve is closed as soon as half the substrate 22 rotation is completed. This ensures complete and uniform coverage of the substrate 22 mounted on the pedestal by the reactive gas or vapor.
  • an inert gas e.g.
  • the substrate 22 is sequentially treated to the pulse from a second type of reactive gas or vapor (e.g. gas/vapor B) through tube 14B that is followed by an inert gas pulse (e.g. P) through tube 14C, each pulse having a width of at least half the substrate 22 rotation.
  • a second type of reactive gas or vapor e.g. gas/vapor B
  • an inert gas pulse e.g. P
  • the substrate 22 holding pedestal rotates through at least two complete rotations. This completes one atomic layer chemical vapor deposition or ALD cycle that is repeated for a desired number of times.
  • the ALD reactor is provided with capabilities for in- situ plasma clean.
  • the RF electrodes 30 consist of flat plates, with coolant channels grooved across their surfaces, that occupy the remnant of the area of the top surface of the reactor.
  • a suitable means of excitation can be applied to these electrodes 30 and a suitable gaseous mixture of gases containing fluorine, chlorine or similar atoms can be injected from the tubes to strike a plasma and generate active species within the reactor.
  • FIG. 5 shows the top view of the ALD reactor with RF electrodes 30 for generating a suitable plasma. Also shown are three gas injector tubes 14 and gas supply lines each with an MFC 18 and a fast switching pneumatic valve 20. The longitudinal apertures 32 in the injector tubes 14 face downward towards the substrate 22 and are shown for the sake of explanation only. The part of the ALD reactor as shown in FIG. 4A, below the cross-section line X-X' remains unchanged.
  • the top portion of the reactor can be opened and is attached to the main body of the reactor with suitable means and an O-ring to maintain vacuum tight seal that is necessary to achieve clean and reproducible processing.
  • the cross-section line X-X' as shown in FIG. 4A separates the lid from the body of the ALD reactor.
  • the body of the reactor may be made of suitable material such as aluminum and/or stainless steel and has a provision for coolant channels within itself so as to maintain the reactor wall temperature constant during processing.
  • the former can be achieved by installing the pneumatic valve 20 as close as possible to the injector tube(s) 14. While later can be achieved by careful optimization of the distance of separation between the tubes 14 or the upper plenum and the substrate plane.
  • the pulse-rotation synchronization mechanism 24 is provided to increase the efficiency of the ALD reactor as shown schematically in FIG. 4A. If the time for one complete substrate rotation around its vertical axis is denoted by T seconds, then the one gas pulse (either reactive or inert) is completed in T/2 seconds. Thus, one complete ALD deposition sequence is completed in 2T seconds as shown in FIG. 6.
  • FIG. 6 shows the gas pulse-rotation synchronization for a typical ALD deposition sequence, where T is the time required for one complete rotation of the substrate around its vertical axis and the Y-axis denotes quantity of the gas at an arbitrary scale and the ALD sequence is shown as [A, P, B, P].
  • Operation of an ALD reactor in CVD mode may also be realized in the event when both the reactive gases and vapor flows A and B are initiated simultaneously by opening the respective pneumatic valves together.
  • the jets emanating from the both the reactive gas or vapor injectors impinge on the diagonal of the substrate, in close vicinity of each other, that is set in angular motion around its axis.
  • FIGS. 4 A and 4B There are several possible variations to the ALD reactor configuration described in FIGS. 4 A and 4B that can achieve atomic layer deposition of thin films. To an individual skilled in the art, however, they are well within the scope of this invention.
  • FIG. 7 shows a top view of an alternative configuration of an ALD reactor with RF electrodes for generating a suitable plasma.
  • a and B constitute reactants but the tube at the center carrying the purge gas P is substituted by bifurcating the purge gas inlet in to two separate purge gas lines 40A and 40B with an individual fast switching pneumatic valve 42 in series, so that purge gas P is supplied to both the reactive gas injector tubes 14A and 14B.
  • the purge gas P adds to the momentum of the reactive gases A and B andit can also help purge the injector tubes and sweep away any excess of either of the reactant accumulated on the substrate.
  • the part of the ALD reactor, as shown in FIG. 4A, below the line X-X' remains unchanged.
  • the ALD deposition sequence in such a configuration can be best described as [A+P, P, B+P, P], However, the process sequence [A, P, B, P] can also be implemented.
  • the top portion of an ALD reactor can be further modified to deposit atomic layers of non-stoichiometric materials such as SixGel-x, or AlxGa(l-x)As. Fabrication of such materials many require as many as four different reactants. These reactants can be categorized in to two sub-groups of reactants that are highly reactive towards each other. For example, one such group of reactants is hydrides and another one is halides of elements such as germanium and silicon.
  • the top of the ALD reactor as described in FIG. 7 can be modified to accommodate the varied number and types of reactants and an inert gas purge as shown in FIG. 8. FIG.
  • FIG. 8 shows the top view of an alternative configuration of an ALD reactor with multiple gas inlets for fabrication of atomic layers of non-stoichiometric materials.
  • the penumatic valves 50 are placed in a bank of three together.
  • the pneumatic block 50 has a common outlet that opens into the injector tubes 14A and 14B.
  • A, B, C and D constitute reactants whereas P is an inert gas purge.
  • the inert gas P can be mixed with the respective reactants upstream as shown by the dashed line.
  • FIG. 9 shows the top view of an alternative configuration of an ALD reactor multiple gas inlets for fabrication of atomic layers of non-stoichiometric materials.
  • Two pneumatic blocks 52 are provided where two pneumatic valves are placed in a bank 52 with minimum dead place.
  • Each pneumatic block 52 has a common outlet that opens in to the injector tubes 14A and 14B, respectively.
  • A, B, C and D constitute reactants whereas P is an inert gas purge that is injected through the injector tube 14C.
  • the gas injector tubes 14 have been largely longitudinal ones in shape. Thus, it is imperative that to achieve complete coverage, the substrate must be rotated through at least 180 degrees.
  • FIGS. 10(a) and 10(b) show a schematic of a cross injector tube 60.
  • FIG. 10(a) shows an individual cross injector 60A with a gas inlet 62 and longitudinal downward slots 64.
  • FIG. 10(b) is a top view of a cross injector 60B having three cross injector tubes 70A, 70B, and 70C combined in close proximity with individual gas inlets.
  • the cross injectors 60 A and 60B can be employed in the top part of an ALD reactor described in detail in FIG. 4A above the line X-X'.
  • FIGS. 11(a) and 11(b) which show a schematic of another ALD reactor configuration in which longitudinal injector tubes are replaced by radial injector tubes 80 that extend inwards from the circumference of a substrate 22 towards and a short distance beyond its center.
  • FIG. 11(a) shows a vertical cross sectional view
  • FIG. 11(b) shows a top view of the ALD reactor with radial tubes 80, injecting on a radius that is directly below the center injector tube.
  • the details of the configuration as shown in FIG. 4A and 4B are omitted for simplicity.
  • the reactants are injected on a rotating substrate 22 from the tubes 80 projecting on the same radius of the largely circular substrate 22 that is set in circular motion at a constant angular speed.
  • the radial injector tubes 80 can be employed in the top part of an ALD reactor described in detail in FIG.-4A above the line X-X'.
  • the length of an injector tube is intentionally made larger than the radius of the substrate in order to provide coverage at the center of the substrate 22.
  • Such an ALD reactor configuration requires that the substrate 22 must be rotated through at least one full rotation during a gas pulse in order to achieve complete coverage by the reactant or purge gas. It is thus imperative that one complete ALD process cycle can be completed through four complete rotations of the substrate 22 around its vertical axis.
  • FIG. 12 shows the Schematic of an ALD reactor with gas injection on a rotating substrate 22 with stacked, peripheral O- rings 90.
  • the details of the configuration as shown in FIG. 4A and 4B are omitted for simplicity.
  • the reactants are injected from circular O-rings 90 placed in individual planes above the substrate 22 and are stacked closely.
  • the O-rings 90 have apertures that project the reactant or purge gas stream on the wafer in such way that it completely covers the substrate 22.
  • the substrate 22 may be rotated to enhance its complete coverage.
  • such an ALD reactor configuration may obviate the substrate rotation as the O-ring 90 injects the gas from all sides on the circular substrate 22.
  • the critical limiting factors, to realize a large area uniform ALD process in such a configuration are mainly the volume of the reactor and path length of the gas (circumference) of the O-rings 90.
  • the volume of the ALD reactor V is defined as follows:
  • V ⁇ (r*2) h (2)
  • r is the radius of the chamber and h is the chamber height. It is also understood that height h of the chamber is closely related to the angle of inclination of the gas stream.
  • the circumference of the ALD reactor L is defined as follows:
  • FIGS. 13(a) and 13(b) show lateral gas injection from stacked and longitudinal gas injectors 100 on a rotating substrate 22.
  • FIG. 13 (a) shows a side view
  • FIG. 13(b) shows a top view of the stacked longitudinal injectors 100.
  • the details of the configuration as shown in FIG. 4A and 4B are omitted for simplicity.
  • the substrate 22 is located approximately midway between the injector tubes 100 that are stacked substantially in a horizontal plane and the exhaust that is situated diametrically at the opposite end of the reactor from the injector tubes 100.
  • the reactants and purge gas jets impinge on the substrate in the vicinity of its diameter.
  • the substrate 22 is set in an angular motion around its vertical axis in horizontal plane during the gas pulses.
  • FIG. 14 shows the schematic of an inverted ALD reactor 106 with stationary
  • the rotation mechanism 108 is placed outside and underneath the ALD reactor 106.
  • the wafer is clamped closely to a heater from behind for efficient heat exchange.
  • the reactants and the purge gas are separately injected into the stationary part of the reactor 106 that is attached to its body.
  • the stationary part in turn feeds each gas into an individual leak-proof rotary feed-through that is attached to each injector tube 110.
  • the injector tubes 110 that are placed in close proximity to each other, and are rotated simultaneously and parallel to each other in a horizontal plane that is substantially parallel to the substrate plane.
  • the reactants subsequent to impinging on the substrate surface 112 flow outwards and depart above and behind the heater from an outlet that is attached to exhaust and/or pump.
  • the substrate be rotated in an inverted ALD reactor 106 configuration with stationary injector tubes at the bottom to inject reactants onto a substrate 112 that is held face down and rotated in a horizontal plane.
  • Such a configuration is exactly similar to the one that is described in detail earlier in FIG. 4, except with one minor difference that it has an additional wafer holding mechanism, such as a vacuum chuck, incorporated within the susceptor.
  • This arrangement enables the operator to hold, rotate and uniformly heat the substrate face down in a horizontal plane during the processing.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

La présente invention concerne un réacteur (13) de dépôt en couches atomiques (atomic layer deposition / ALD) comprenant un compartiment essentiellement cylindrique (15) et un substrat en tranche (22) fixé à l'intérieur du compartiment (15). Le réacteur ALD (13) comprend également au moins un tube d'injection (14) monté à l'intérieur du compartiment (15) doté d'une pluralité d'ouvertures (32) situées le long d'une face, servant à diriger le gaz émanant des ouvertures (32) vers le substrat en tranche (22). Lorsque le gaz est expulsé du tube d'injection (14), soit le substrat en tranche (22), soit le tube d'injection (14) tourne de façon continue dans un plan longitudinal à l'intérieur du compartiment (15) de sorte que le gaz recouvre complètement et uniformément le substrat en tranche (22).
PCT/US2000/017202 1999-06-24 2000-06-23 Dispositif de depot chimique en couches atomiques en phase vapeur WO2000079019A1 (fr)

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Application Number Priority Date Filing Date Title
EP00950239A EP1226286A4 (fr) 1999-06-24 2000-06-23 Dispositif de depot chimique en couches atomiques en phase vapeur
JP2001505362A JP2003502878A (ja) 1999-06-24 2000-06-23 原子層化学気相成長装置
US10/019,244 US6812157B1 (en) 1999-06-24 2000-06-23 Apparatus for atomic layer chemical vapor deposition
AU63367/00A AU6336700A (en) 1999-06-24 2000-06-23 Apparatus for atomic layer chemical vapor deposition
US10/865,111 US20040224504A1 (en) 2000-06-23 2004-06-09 Apparatus and method for plasma enhanced monolayer processing

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US14111199P 1999-06-24 1999-06-24
US60/141,111 1999-06-24

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US10/370,883 Continuation-In-Part US20040129212A1 (en) 2002-05-20 2003-02-21 Apparatus and method for delivery of reactive chemical precursors to the surface to be treated

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EP1357583A4 (fr) * 2001-01-09 2005-05-25 Tokyo Electron Ltd Dispositif de traitement a feuilles
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US9012334B2 (en) 2001-02-02 2015-04-21 Applied Materials, Inc. Formation of a tantalum-nitride layer
US9587310B2 (en) 2001-03-02 2017-03-07 Applied Materials, Inc. Lid assembly for a processing system to facilitate sequential deposition techniques
WO2002070779A1 (fr) * 2001-03-02 2002-09-12 Applied Materials, Inc. Appareil et procede de depot sequentiel de films
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US6620670B2 (en) 2002-01-18 2003-09-16 Applied Materials, Inc. Process conditions and precursors for atomic layer deposition (ALD) of AL2O3
US6827978B2 (en) 2002-02-11 2004-12-07 Applied Materials, Inc. Deposition of tungsten films
US6833161B2 (en) 2002-02-26 2004-12-21 Applied Materials, Inc. Cyclical deposition of tungsten nitride for metal oxide gate electrode
US6720027B2 (en) 2002-04-08 2004-04-13 Applied Materials, Inc. Cyclical deposition of a variable content titanium silicon nitride layer
US6861094B2 (en) 2002-04-25 2005-03-01 Micron Technology, Inc. Methods for forming thin layers of materials on micro-device workpieces
US6838114B2 (en) 2002-05-24 2005-01-04 Micron Technology, Inc. Methods for controlling gas pulsing in processes for depositing materials onto micro-device workpieces
US7118783B2 (en) 2002-06-26 2006-10-10 Micron Technology, Inc. Methods and apparatus for vapor processing of micro-device workpieces
US6821347B2 (en) 2002-07-08 2004-11-23 Micron Technology, Inc. Apparatus and method for depositing materials onto microelectronic workpieces
US7357138B2 (en) 2002-07-18 2008-04-15 Air Products And Chemicals, Inc. Method for etching high dielectric constant materials and for cleaning deposition chambers for high dielectric constant materials
US7754013B2 (en) 2002-12-05 2010-07-13 Asm International N.V. Apparatus and method for atomic layer deposition on substrates
US9121098B2 (en) 2003-02-04 2015-09-01 Asm International N.V. NanoLayer Deposition process for composite films
US8658259B2 (en) 2003-02-04 2014-02-25 Asm International N.V. Nanolayer deposition process
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US7055263B2 (en) 2003-11-25 2006-06-06 Air Products And Chemicals, Inc. Method for cleaning deposition chambers for high dielectric constant materials
US8518184B2 (en) 2003-12-10 2013-08-27 Micron Technology, Inc. Methods and systems for controlling temperature during microfeature workpiece processing, E.G., CVD deposition
US8384192B2 (en) 2004-01-28 2013-02-26 Micron Technology, Inc. Methods for forming small-scale capacitor structures
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US7189287B2 (en) 2004-06-29 2007-03-13 Micron Technology, Inc. Atomic layer deposition using electron bombardment
US7628855B2 (en) 2004-06-29 2009-12-08 Micron Technology, Inc. Atomic layer deposition using electron bombardment
US9032906B2 (en) 2005-11-04 2015-05-19 Applied Materials, Inc. Apparatus and process for plasma-enhanced atomic layer deposition
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US20130237063A1 (en) * 2012-03-09 2013-09-12 Seshasayee Varadarajan Split pumping method, apparatus, and system
CN107815668A (zh) * 2017-12-05 2018-03-20 南京工业大学 一种面向中空纤维膜批量改性的旋转原子层沉积反应器
CN107815668B (zh) * 2017-12-05 2023-05-23 南京工业大学 一种面向中空纤维膜批量改性的旋转原子层沉积反应器
CN114072538A (zh) * 2019-04-25 2022-02-18 Beneq有限公司 前驱体供应柜
CN114072538B (zh) * 2019-04-25 2023-08-22 青岛四方思锐智能技术有限公司 前驱体供应柜

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EP1226286A1 (fr) 2002-07-31
AU6336700A (en) 2001-01-09
EP1226286A4 (fr) 2007-08-15
JP2003502878A (ja) 2003-01-21

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