Bottom fed sublimation bed for high saturation efficiency in semiconductor applications

Ampoules for a semiconductor manufacturing precursors and methods of use are described. The ampoules include a container with an inlet port an outlet port, a manifold having a serpentine base creating a tortuous flow path and a filter media assembly in a bottom-fed configuration. The torturous flow path is defined by a plurality of elongate walls and a plurality of openings of the serpentine base ampoule, through which a carrier gas flows in contact with the precursor.

TECHNICAL FIELD

The present disclosure relates generally to ampoules and methods for using ampoules for semiconductor manufacturing precursors. In particular, the disclosure relates to ampoules and methods to provide bottom fed sublimation bed and tortuous flow path for low vapor pressure precursors.

BACKGROUND

The semiconductor industry is using an increasing variety of chemistries for chemical vapor deposition (CVD) and atomic layer deposition (ALD) processes that come in liquid or solid form. The precursor is typically inside a closed vessel or ampoule with a single inlet and a single outlet.

Solid precursors with a low vapor pressure frequently use a carrier gas to carry the vapor out of the ampoule to the process reactor. For these types of processes there are two types of ampoules typically used: a bubbler where the inlet carrier gas goes into a tube that is submerged into the precursor; and a cross-flow ampoule where the carrier gas sweeps headspace in the ampoule from the top. Often, there is only a very short flow path for the carrier gas. The short flow path from the inlet to the outlet of the vessel does not allow adequate residence time within the vessel to allow the carrier gas to become fully saturated with vaporized or sublimed precursor. Some existing ampoule designs do not evenly distribute the carrier gas across the entire surface of the precursor. Some existing ampoules designs do not provide adequate heating of the precursor within the entire vessel. Many other solid source ampoules do not provide a means for keeping precursor dust from traveling downstream where it hampers control valve performance or creates on-wafer particle issues.

Conventional top-fed sublimation architectures include an ampoule or canister partially filled with solid precursor, which rests on the bottom of the ampoule. As the ampoule is heated and carrier gas is introduced into the head space of the ampoule, sublimation occurs between the top surface of the solid precursor and the carrier gas within the head space. In an ideal scenario, the carrier gas flowing through the ampoule becomes saturated with the precursor. As the head space of the ampoule increases, resulting in varying concentrations of saturated carrier gas, an inconsistent dose of precursor-carrier gas is supplied. As such, carrier gas saturation is not maintained due to inefficiencies in the ampoule and solid precursor depletion.

There is a need in the art for ampoules, methods of making ampoules and/or methods of using ampoules with one or more of an increased flow path, increased surface area for sublimation and for consistent concentrations of saturated carrier gas.

SUMMARY

One or more embodiments are directed to an ampoule for a semiconductor precursor material having a torturous path for increased dwell time in a bottom-fed configuration. The ampoule comprises a container, a lid, a manifold inserted into the container and a filter media on which precursor material rests.

The container has a bottom wall and sidewalls defining a precursor cavity configured to hold the precursor material. The lid is in contact with the sidewalls and the lid has an inlet port and an outlet port extending through the lid. The manifold comprises a hollow cylindrical shaft with an outlet and a serpentine base positioned at a bottom end of the shaft, the serpentine base has a top surface and a bottom surface, the bottom surface has a plurality of elongate walls extend therefrom, each of the elongate walls having a plurality of openings in adjacent elongate walls off-set from one another forming a torturous flow path.

The filter media assembly is in contact with the bottom end of the shaft forming a sublimation cavity between a bottom surface of the filter media assembly and the top surface of the bottom wall, the sublimation cavity including the bottom end of the shaft and the serpentine base. An inlet conduit extends from the lid to the sublimation cavity, so that a gas flowing through the inlet conduit passes through the torturous path and out the outlet in the hollow cylindrical shaft.

In some embodiments, the precursor material rests on the filter media assembly such that depletion of solid precursor does not cause concentration variations within the sublimation cavity. The filter media assembly comprises a first filter media and a frame, the first filter media having a porosity such that vaporized precursor can pass through. The material is heated such that a vapor precursor is formed and flows through the filter media assembly and is mixed and sublimed with carrier gas.

In some embodiments, the ampoule further comprises a gas ring in fluid communication with the inlet port, the gas ring comprising a plurality of outlet holes configured to allow a carrier gas to pass through the gas ring. The gas ring positioned below the filter media assembly such that carrier gas is distributed across a bottom surface of the filter media assembly. In some embodiments the gas ring is connected to the inlet port by an inlet conduit, while in other embodiments the gas ring is integral to the bottom end of the shaft.

In some embodiments, the manifold further comprises a top wall having an integral inlet port in fluid communication with the hollow shaft and the gas ring, so that a carrier gas can pass through the shaft and out of the outlet holes and across the filter media assembly. In some embodiments, the outlet port is in fluid communication with a central cavity of the serpentine base, the central cavity bounded by an innermost wall of the plurality of walls, and the bottom wall of the container. In some embodiments, central cavity is in fluid communication with the outlet port via an outlet conduit and the outlet conduit is in fluid communication with an integral outlet port formed in the top wall of the manifold. In some embodiments, the central cavity is in direct communication with the hollow shaft such that gases are exhausted through the shaft and to the outlet port. In some embodiments, the manifold further comprises an integral outlet conduit and an integral electrical conduit and the inlet port is in fluid communication with the hollow shaft such that carrier gas is distributed from the shaft through an integral gas ring.

Further embodiments comprise a manifold having a base with a top surface and a bottom surface, the bottom surface having a plurality of elongate walls extending therefrom, each of the elongate walls having a plurality of openings with openings in adjacent elongate walls off-set from one another forming a torturous flow path defining a bottom exchange zone, and the top surface also having a plurality of elongate walls extending therefrom defining an upper exchange zone.

In the appended figures, similar components and/or features may have the same reference label. Further, various components of the same type may be distinguished by following the reference label by a dash and a second label that distinguishes among the similar components. If only the first reference label is used in the specification, the description is applicable to any one of the similar components having the same first reference label irrespective of the second reference label. The cross-hatch shading of the components in the figures are intended to aid in visualization of different parts and do not necessarily indicate different materials of construction.

DETAILED DESCRIPTION

Some embodiments of the disclosure advantageously provide a long flow path for a carrier gas from ampoule inlet to outlet for the delivery of low vapor pressure precursors, e.g., liquid and/or solid source precursor. Low vapor pressure precursors are understood to refer to materials that do not readily vaporize under atmospheric conditions. Low vapor pressure precursors typically have a vapor pressure of less than 10 Torr, and more typically less than 1 Torr. In some applications, a carrier gas is used to deliver low vapor pressure material from an ampoule to a reactor. Low vapor pressure materials typically require heat to increase the vapor pressure. A non-limiting list of exemplary precursors includes ZrCl4, Y(EtCP)3, HfCl4, WCl5, MoCl5, In(CH3)3, and liquid Silo, Mg(Cp)2.

A flow path having a long and torturous distance allows the carrier gas adequate residence time to become partially to nearly to fully saturated with vaporized and/or sublimed and/or entrained precursor. As used herein, the term “torturous path” means a flow path that has multiple branches, curves, angles, turns, etc., that prevent a straight path for the flow. In some embodiments, the torturous path increases the residence time of the gas within the manifold to increase concentration uniformity. Reference herein to “saturated” allows for varying degrees of saturation.

Some embodiments of the disclosure advantageously provide bottom-fed ampoule configurations. Some embodiments advantageously provide ampoules in which depletion of the solid precursor does not affect the concentration of the saturated carrier gas.

Some embodiments provide apparatus and methods for heating low vapor pressure precursors in large volume ampoules, including ways to provide effective uniform heating of the precursors. Some specific embodiments advantageously retain low vapor pressure precursors, including solid precursor dust, within a cavity of the vessel, not allowing it to migrate upstream or downstream to control valves by means of filter media. Some embodiments advantageously control uneven depletion of the precursor. Some embodiments advantageously provide even distribution of the carrier gas along the entire surface of a precursor bed in a bottom-fed configuration. Embodiments herein provide improved doses of the precursor.

In some embodiments, the ampoules comprise a removable manifold having a plurality of elongate walls defining a labyrinth such that the flow path is tortuous. Advantageously, one or more embodiments provide a flow path whose distance can be five to ten times longer than distances found with common ampoules, in particular solid source sublimation vessels. The increased flow path allows for a longer dwell time of carrier gas and vaporized precursor chemistry to mix within the ampoule.

Ampoules disclosed herein comprise a container defining a cavity configured to hold a precursor; an inlet port and an outlet port, both in fluid communication with the cavity; and a removable manifold having a serpentine base. The serpentine base comprises a plurality of elongate walls arranged to define torturous flow channels (also referred to a “serpentine path”), each of the elongate walls comprising a plurality of openings opening. A flow path is defined by the flow channels and the plurality of openings, through which a carrier gas flows in contact with the precursor. In some embodiments, the serpentine base comprises a plurality of top elongate walls extending from a top surface of the serpentine base and a plurality of bottom elongate walls extending from a bottom surface of the serpentine base. The plurality of top elongate wall and plurality of bottom elongate walls each define torturous flow paths such that the dwell time of the carrier gas and vaporized precursor chemistry is increased within the ampoule. In one or more embodiments, the flow path travels from an outermost channel to an innermost channel, which may be referred to as an “outer-to-inner flow” configuration. In one or more embodiments, the flow path travels from an innermost channel to an outermost channel, which may be referred to as an “inner-to-outer flow” configuration. In some embodiments, carrier gas has an inner-to-outer flow through the plurality of top elongate walls and subsequently has an outer-to-inner flow through the plurality of bottom elongate walls.

Ampoules disclosed herein are in a bottom-fed configuration such that the precursor is separated from a lower chamber by a sublimation bed. In such a configuration, the lower chamber maintains a constant volume as precursor resting above the sublimation bed is depleted as carrier gas passes across the one or more filter media. The lower chamber of the ampoule is separated into an upper exchange zone and a lower exchange zone. The upper exchange zone is a volume between the sublimation bed and the top surface of the serpentine base, and the lower exchange zone is a volume between the bottom surface of the serpentine base and the inner surface of the bottom wall of the container. Each upper exchange zone and lower exchange zone is configured to increase the dwell time of carrier gas and vaporized precursor chemistry to mix within the ampoule.

Carrier gas passes across the sublimation bed in the upper exchange zone where the precursor chemistry and the carrier gas flow to form a saturated gas mixture of precursor and carrier gas. Carrier gas is streamed directly across the filter media in order to saturate the carrier gas with precursor particles. In some embodiments, the carrier gas flows through a torturous path positioned within the upper exchange zone. The torturous path is configured to increase the duration in which the carrier gas is interacting with precursor chemistry within the upper exchange zone. While still within the lower chamber, the saturated gas then passes through a “lower exchange zone” also comprising a torturous path before exiting the lower chamber and the ampoule. In some embodiments, the filter media comprises a mesh with a pore size sufficient to prevent solid precursor from passing through.

In some embodiments, the manifold is configured to provide an internal heat source for controlling temperature within the ampoule in accordance with precursor sublimation chemistries. In some embodiments, heating elements are disposed on the exterior of the ampoule. In some embodiments, a cable heater is integral or brazed between two plates positioned between the upper and lower exchange zones such that gases flowing within the upper and lower exchange zones are heated, promoting both sublimation of the precursor material and saturation of the carrier gas.

Generally, the flow paths provided herein force the carrier gas to flow around a series of elongate walls, which in one or more particular embodiments are nested concentric tubes having one or more plurality of openings passageways, which define flow channels. The gas flow changes direction from flow channel to flow channel until the last flow channel in communication with the outlet port is reached. This change of direction also enhances mixing of the vaporized and/or sublimed precursor with the carrier gas. Plurality of openings allow the carrier gas to flow through into the next flow channel creating a torturous path. As the carrier gas passes from an inlet through the upper exchange zone, lower exchange zone and through the outlet, pure carrier gas becomes partially saturated and then fully saturated with precursor chemistry before exiting through the outlet.

Reference herein to gas flow includes the carrier gas alone or in combination with entrained and/or vaporized and/or sublimed precursor. The flow paths of the upper and lower exchange zones described herein, for example, inFIGS.5A,5B,5C,9A,9B and11, comprise a series of elongate walls, tubular or otherwise, with plurality of openings configured to define flow channels therebetween will result in a desired flow path. In some embodiments, the plurality of openings are off-set to ensure no flow channels are bypassed. Such a configuration is referred throughout the disclosure as “serpentine path” or “torturous path” interchangeably.

FIGS.1through3Aillustrate schematic representations of an ampoule and an accompanying manifold having a bottom fed configuration in accordance with embodiments of the present disclosure. Similarly,FIGS.4,6,7,9A and9Billustrate side views and perspective views of the ampoule and the accompanying manifold.FIG.3Billustrates a side view of a filter media in accordance with an embodiment of the present disclosure.FIGS.4through11illustrate an ampoule and an accompanying manifold withFIGS.5A-5C,8,10and11illustrating the manifold in accordance with embodiments of the present disclosure. An ampoule having a manifold are suitable for use with semiconductor manufacturing raw materials, which include reagents and precursors. In the embodiments shown, the precursor is suspended above a sublimation bed having a filter media. The general region below the sublimation bed is characterized as a lower chamber in which saturation of the carrier gas occurs. Pure or unsaturated carrier gas first passes from the manifold across the sublimation bed of the upper exchange zone where the precursor chemistry and the carrier gas flow to form a saturated gas mixture of precursor and carrier gas. While still within the lower chamber, the saturated gas then passes through a lower exchange zone also comprising a torturous path before exiting the lower chamber and the ampoule. The term “precursor” is used to describe the contents of the ampoule and refers to any reagent that flows into a process environment.

The ampoule100includes a container102with a bottom wall104, sidewalls106, and a lid116. An inlet port120and outlet port130are in fluid communication with a precursor cavity140defined by internal walls107of the container102. The inlet port120is generally configured to allow a connection to a gas source “G” by way of suitable piping and valve(s) and may have suitable threaded or sealing connections. In one or more embodiments, the gas source “G” is a carrier gas; in one or more embodiments, the carrier gas is inert, such as N2, Ar or He; in one or more embodiments, the carrier gas is not inert, such as H2, provided the carrier gas doesn't react with precursor in vessel. The outlet port130is also in fluid communication with the precursor cavity140. The outlet port130is generally configured to be able to connect to a line, including suitable piping and valve(s), to allow the flow of gases, which may include entrained particles, exiting the container102to flow to a processing chamber (or other component). The inlet port120and the outlet port130may have a welded or threaded connection to allow a gas line to be connected. While the embodiments depict one of each an inlet and an outlet port, should a particular application require, multiple inlet ports and outlet ports may be present.

In the figures, a flow path is generally indicated by a series of dashed arrows showing the gas source “G” starting from the inlet port120and exiting through the outlet ports130. In some embodiments, as best shown inFIGS.4-5, the inlet port120and outlet port130are integral to the manifold250(represented as integral inlet port246and an integral outlet port247of the manifold250which are in fluid communication with inlet port220and an outlet port230of the lid216). In some embodiments, as best shown inFIGS.1-3A, the inlet port120is separate from the manifold150.

As shown inFIG.1, a height “H” of the precursor cavity140defined by the container102spans from a bottom surface117of the lid116to a top surface105of the bottom wall104.

With reference toFIGS.1-3A, the manifold150comprises a hollow cylindrical shaft152having a top end154and a bottom end156, and a serpentine base160integral to the bottom end156of the cylindrical shaft152. In some embodiments, the cylindrical shaft152and serpentine base160are a unitary body. In some embodiments, the cylindrical shaft152and serpentine base160are welded, threaded or otherwise affixed together by conventional means. In the illustrated embodiments, the top end154of the manifold150functions as the outlet port130where sublimed carrier gas exits the manifold150and the ampoule100.

The serpentine base160comprises a top surface164and a bottom surface166. From the bottom surface166extend a plurality of elongate walls168defining a plurality of flow channels272(as best shown inFIG.11). In some embodiments, the elongate walls168are in contact with the top surface105of the bottom wall104of the container102.

As best shown inFIGS.3A,5B,5C,10and11, The elongate walls (168,268,368,394) each comprise an plurality of openings (169,269,369) forming a torturous flow path signified by the arrows in the figures. The elongate walls (168,268,368,394) and the plurality of openings (169,269,369) together form a maze-like or “zig-zag” torturous flow path such that not one plurality of openings opening overlaps with another plurality of openings. By way of example, sublimed gas G enters from an plurality of openings (169,269) of an outermost elongate wall (168a,268a) and exits from an plurality of openings (169,269) to an innermost elongate wall268b. Stated differently, the plurality of openings (169,269) of any of the elongate walls (168,268) is offset from an adjacent elongate wall (168,268).

A flow path of the bottom surface166of the serpentine base160(the lower exchange zone) is defined as follows: carrier gas G enters through the plurality of openings169of the outermost wall (168a,268a) through subsequent elongate walls (168,268) until the carrier gas G has reached the plurality of openings169of the innermost wall (168b,268b). As carrier gas G passes through the plurality of openings169of the innermost wall (168b,268b), it enters a central cavity170after which the carrier gas G is exhausted, as explained in further detail below. The central cavity170is defined by an inner surface of the innermost wall (168b,268b), the bottom surface166of the serpentine base160and the top surface105of the bottom wall104of the container102.

As shown inFIGS.1and3A, in some embodiments, the hollow cylindrical shaft152is in fluid communication with the central cavity170through a centrally located passage162of the serpentine base160. In some embodiments, the passage162has a diameter which is substantially equal to an inner diameter of the hollow cylindrical shaft152such that gases can have an uninterrupted flow. In some embodiments, as shown inFIG.2, an outlet conduit131of the outlet port130is in fluid communication with the central cavity170. In both embodiments, carrier gas G is exhausted from the central cavity170to the outlet port130.

As shown inFIGS.1-3A, the ampoule further comprises a filter media assembly180(also characterized as a “sublimation bed”) comprising a frame182and a first filter media184in the form of a planar disk. The first filter media184is concentric to the hollow cylindrical shaft152of the manifold150. The first filter media184has a top surface188and bottom surface189and has a porosity such that vaporized precursor may pass through but liquid or solid precursor may not. In some embodiments, first filter media184has a porosity in the range of 0.2 to 3000 μm, or in the range of 0.5 to 2500 μm, or in the range of 1 to 2000 μm Microns.

The filter media assembly180has a planar disk shape and is positioned around the cylindrical shaft152of the manifold150and the inner walls107of the container102. In particular, the frame182which holds the first filter media184extends from the cylindrical shaft152to the inner walls107. As shown inFIG.1, in some embodiments, the frame182rests on the top surface164of the serpentine base160. As shown inFIG.2, in some embodiments, the frame182rests on a gas ring190. As shown inFIG.3A, in some embodiments, the filter media assembly180only consists of a first filter media184, and the first filter media184rests on both the gas ring190and an inner ledge108of the internal walls107. In some embodiments, the frame182of the filter media assembly180is fastened or secured to the inner ledge108by an outer retention ring. In some embodiments, the frame182of the filter media assembly180is fastened or secured to the top surface164of the serpentine base160by an inner retention ring.

A sublimation cavity142is defined by the bottom surface189of the first filter media184and filter media assembly180, the bottom end156of the cylindrical shaft152, the internal walls107and the top surface105of the bottom wall104of the container102. Above the top surface188of the filter media, a low vapor pressure material144(referred to as a “precursor” or “precursor material”) is within the precursor cavity140, residing above the filter media assembly180. Space above the material144within the precursor cavity140is a dead space of the ampoule100. As the material144depletes, the volume of the dead space increases without affecting the concentration of the saturated or partially saturated carrier gas within the lower chamber due to the volume of the lower chamber remaining constant. The material144can be a precursor for use with a semiconductor manufacturing process. In one or more embodiments, the material with a low vapor pressure is a solid.

As the ampoule100is heated, the material144vaporizes creating a saturated vaporized precursor within the precursor cavity140. As explained in further detail below, as carrier gas passes across the first filter media184within the upper exchange zone, it mixes with vaporized precursor material144present in the upper exchange zone of the sublimation cavity142. Heating the ampoule100causes the material144in intimate or proximate contact with the first filter media184to sublime and diffuse across and through the first filter media184into the sublimation cavity142, and in particular the upper exchange zone. The sublimed material144saturates the carrier gas after passing through the first filter media184. In some embodiments, the dead space above the precursor material144can contain sublimed material144in vapor form.

As shown inFIG.3A, in some embodiments, the filter media assembly180further comprises a plurality of filter cylinders186extending from the top surface188of the first filter media184. The filter cylinders186are configured to increase surface area of the first filter media184. In some embodiments, the filter cylinders186further comprise an internal conduit187extending the length of the filter cylinders186such that carrier gas may flow through the filter cylinders186thereby increasing the surface area.

In the embodiments shown inFIGS.1-3A, carrier gas G enters the container102from the inlet port120. The inlet port is in fluid communication with the sublimation cavity142by an inlet conduit122. As shown inFIG.1, in some embodiments, the inlet conduit122is connected to an outer portion of the frame182. As shown inFIGS.2and3A, in some embodiments, the inlet conduit122is connected to a gas ring190surrounding the bottom end156of the manifold150. In both configurations, the carrier gas G is directed across the first filter media184such that vaporized precursor passing through the first filter media184is carried and mixed with the carrier gas G.

In some embodiments, the gas ring190comprises a ring-shaped body surrounding the bottom end156of the manifold. The gas ring190includes a ring-shaped internal channel having a plurality of outlet holes192configured to expel carrier gas G from the gas ring190. The gas ring190is connected to the inlet port120such that carrier gas G from the inlet port120is distributed and ejected across the first filter media184.

A flow path of the entire ampoule100is defined as follows: carrier gas G enters the ampoule100and is distributed across the filter media184via the gas ring190of some embodiments, or directly from the inlet conduit122of some embodiments. As the carrier gas G enters the sublimation cavity142and is distributed across the filter media184, vaporized precursor which is passing through the first filter media184is carried and mixed with the carrier gas G. Due to the diameter of the serpentine base160being smaller than the diameter of the inner walls107of the container102, the mixture of carrier gas G and vaporized precursor surrounds the serpentine base160and enters through the plurality of openings169of the outermost wall (168a,268a) through subsequent elongate walls (168,268) until the gases have reached the plurality of openings169of the innermost wall (168b,268b). As the gases pass through the plurality of openings169of the innermost wall (168b,268b), the gas enters a central cavity170after which the gases are exhausted.

Because the material144is fed through the filter media assembly180in a bottom fed configuration, depletion of material144does not cause concentration variations within the sublimation cavity142.

As shown inFIG.1, in some embodiments, the cylindrical shaft152itself is configured as an outlet port, where the gasses are exhausted directly from the central cavity170. As shown inFIG.2, in embodiments having the outlet conduit131extending through the cylindrical shaft152, electrical or control wires can be positioned within the cylindrical shaft152as gases do not come into contact with the electrical or control wires.

As shown inFIGS.1-3, in some embodiments, an auxiliary port137extends through the lid170and is in fluid communication with the central cavity170. The auxiliary port137according to some embodiments is used for purging, charging with inert gas, or for leak testing.

In some embodiments, a fine filter media (183,283) is positioned within the cylindrical shaft152such that fine particles and/or droplets of precursor do not exit the ampoule. In some embodiments, the fine filter media (183,283) may be any suitable material or configuration or dimensions or media grade offering one or more of the following characteristics: withstands long-term exposure to the precursor, does not introduce a pressure drop that would impede effective delivery of the precursor, pore size to inhibit and/or prevent fine particles and/or droplets of precursor from exiting the ampoule to protect outlet equipment, and pliable to be capable of making a slight seal with the cylindrical shaft. A non-limiting, exemplary porosity of the fine filter media (183,283) may be greater than or equal to 0.1 micrometers to less than 100 micrometers, and all values and subranges therebetween, as measured by average pore size.

In some embodiments, as best shown inFIG.2, the ampoule100further comprises one or more external heating elements134positioned in one or more of the bottom wall104, the sidewalls106and the lid116. In some embodiments, as best shown inFIG.2, the manifold150further comprises an internal heating element136positioned and in contact with the top surface164of the serpentine base160. In some embodiments, a cable heater is integral or brazed between the upper and lower exchange zones such that gases flowing within the upper and lower exchange zones are heated, promoting both sublimation of the precursor material and saturation of the carrier gas. The one or more external heating elements134are configured to vaporize the material144within the precursor cavity and the internal heating element136is configured to heat the serpentine base160and the elongate walls168to promote sublimation of the vapor precursor and carrier gas G throughout the sublimation cavity142.

FIGS.4-5C, illustrate a manifold350in accordance with one or more embodiments having a plurality of bottom elongate walls368extending from a bottom surface366of a serpentine base360and a plurality of top elongate walls394extending from a top surface364of the serpentine base360. The plurality of bottom elongate walls368and the plurality of top elongate walls394each independently define a plurality of flow channels272(as best shown inFIG.11).

The manifold350comprises an integral inlet port320, outlet port330and gas ring390. The manifold350comprises a hollow cylindrical shaft352having a top end354and a bottom end356, and the serpentine base360integral to the bottom end356of the cylindrical shaft352. In some embodiments, the cylindrical shaft352and serpentine base360are a unitary body. In some embodiments, the cylindrical shaft352and serpentine base360are welded, threaded, or otherwise affixed together by conventional means. In the illustrated embodiments, the top end354of the manifold350comprises a top wall345having an integral inlet port346and an integral outlet port347. The integral inlet port346and an integral outlet port347of the top wall345are in fluid communication with an inlet port320and an outlet port330of the lid316. The integral outlet port247is in fluid communication with the cylindrical shaft252itself.

Carrier gas G entering from the inlet port320and the integral outlet port347passes into the cylindrical shaft352and exits across the filter media assembly380by way of the integral gas ring390. As best shown inFIG.5A, the gas ring390is a flange extending outward from the bottom end356of the manifold350. The gas ring390further includes a plurality of outlet holes392configured to expel carrier gas G from the gas ring390across the filter media assembly380. In some embodiments, the plurality of outlet holes392are parallel to the filter media, expelling carrier gas G directly across the filter media.

In the depicted embodiment, the plurality of outlet holes392expel carrier gas G into a plurality of openings369of an innermost elongate wall394aof the plurality of top elongate walls394and through the torturous path formed by the plurality of top elongate walls394. As the carrier gas G passes through each elongate wall of the plurality of top elongate walls394, it mixes with vaporized precursor material which is passing through a medium filter media383. The mixture of carrier gas G and vaporized precursor material exits through a plurality of openings369of an outermost elongate wall394b. The mixture of carrier gas G and vaporized precursor surrounds the serpentine base360and enters through the plurality of openings369of an outermost wall368athrough subsequent elongate walls until the gases have reached the plurality of openings369of the innermost wall368b. As the gases pass through the plurality of openings369of the innermost wall368b, the gas enters a central cavity370after which the gases are exhausted.

With reference toFIG.5A, some embodiments of the disclosure are directed to base360for a manifold350. The base360of some embodiments, as illustrated, has a top surface364with a plurality of walls with an innermost elongate wall394aand an outermost elongate wall394b. In some embodiments, there are one or more intermediate elongate walls between the innermost elongate wall394aand the outermost elongate wall394bto provide a plurality of concentric channels on the top surface364of the base360. Each of the elongate walls has at least one opening369to allow fluid communication between adjacent channels on the top of the base. The base360also includes a bottom surface366with a plurality of walls with an innermost elongate wall368band an outermost elongate wall368a. In some embodiments, there are one or more intermediate elongate walls between the innermost elongate wall368band the outermost elongate wall368ato provide a plurality of concentric channels on the bottom surface366of the base360. Each of the elongate walls has at least one opening369to allow fluid communication between adjacent channels on the bottom of the base.

FIGS.6-10illustrate a manifold250in accordance with one or more embodiments having an integral inlet port220, outlet port230and gas ring290. The manifold250comprises a hollow cylindrical shaft252having a top end254and a bottom end256, and a serpentine base260integral to the bottom end256of the cylindrical shaft252. In some embodiments, the cylindrical shaft252and serpentine base260are a unitary body. In some embodiments, the cylindrical shaft252and serpentine base260are welded, threaded or otherwise affixed together by conventional means.

In the illustrated embodiments, the top end254of the manifold250comprises a top wall245having an integral inlet port246and an integral outlet port247. The integral inlet port246and an integral outlet port247of the top wall245are in fluid communication with an inlet port220and an outlet port230of the lid216. The integral outlet port247is in fluid communication with the cylindrical shaft252itself.

Carrier gas G entering from the inlet port220and the integral outlet port247passes into the cylindrical shaft252and exits across the filter media assembly280by way of the integral gas ring290. As best shown inFIGS.9A,9B and8, the gas ring290is a flange extending outward from the bottom end256of the manifold250. The gas ring290further includes a plurality of outlet holes292configured to expel carrier gas G from the gas ring290across the filter media assembly180.

After the vaporized precursor and carrier gas G pass through the serpentine base260as previously explained, the gas mixture exits the manifold through an integral outlet conduit248which extends from the serpentine base260to the integral outlet port247and the outlet port230.

In some embodiments, the manifold further comprises a fine filter media283positioned at the integral outlet conduit248, preventing fine particles and/or droplets of precursor from exiting the ampoule100. In some embodiments, the fine filter media283may be any suitable material or configuration or dimensions or media grade offering one or more of the following characteristics: withstands long-term exposure to the precursor, does not introducing a pressure drop that would impede effective delivery of the precursor, pore size to inhibit and/or prevent fine particles and/or droplets of precursor from exiting the ampoule to protect outlet equipment, and pliable to be capable of making a slight seal with the cylindrical shaft. A non-limiting, exemplary porosity of the fine filter media283may be greater than or equal to 0.1 micrometers to less than 100 micrometers, and all values and subranges therebetween, as measured by average pore size.

In some embodiments, as best shown inFIG.6, the manifold250further comprises an integral electrical conduit249extending from serpentine base260to an integral conduit port (not shown) of the manifold250and an electrical conduit port of the lid226. In some embodiments, the integral electrical conduit249houses signal, electrical or metrology cables.

Where the manifold250comprises integral inlet and outlet ports, the entire manifold250can be removed for ease of cleaning the ampoule100. In some embodiments, the manifold250is dimensioned to fit within a conventional container ampoule. Thus, the manifold250can slide down into position such that the elongate walls268come into contact with the bottom wall104of the ampoule. An appropriately sized filter media assembly180can then be positioned into the container102and the lid216can seal the container102. Thus, fastening of gas or electrical conduits is not necessary, reducing assembly time.

In some embodiments, each of the aforementioned structures which come into contact with one another further comprise circular channels for the placement of O-rings or other sealants. In particular, in some embodiments, one or more O-rings is positioned between the filter media assembly180and the cylindrical shaft (152,252), and between the filter media assembly180and the sidewalls106. In some embodiments, O-rings are positioned between the sidewalls106and the bottom surface of the lid (116,216), and between the top wall of the manifold250) and the bottom surface of the lid216. In some embodiments, as best shown inFIG.1, O-rings are positioned between the shaft152and an inner surface of an aperture of the lid116through which the shaft extends through.

In some embodiments, the ampoule100is stored and transported up-side-down such that the material144rests on the bottom surface117of the lid116. In such a configuration, damage to the filter media assembly180is prevented, and migration of the material144through the filter media assembly180is prevented.

In some embodiments, components are connected using removable bolts through appropriately shaped openings, which may have a threaded portion to allow for easy connection of a threaded bolt. The bolts can be removed to allow disassembly.

In some embodiments, as best shown inFIG.7, a plurality of grooves109are formed in the bottom wall such that the plurality of grooves can interdigitate with the elongate walls168, forming a seal which prevents passage of gases underneath the elongate walls168.

According to one or more embodiments, the plurality of openings of any embodiment are suitable to allow carrier gas to flow from one flow channel to another. The plurality of openings may take any suitable shape and/or configuration and/or location along the elongate walls to accommodate flow of entrained and/or saturated carrier gas. Features of the plurality of openings could be a plurality of holes, tapered slots, or other shapes. In one or more embodiments, the plurality of openings are sized and shaped to provide a varying conductance of carrier gas along a longitudinal distance of the container. In one or more embodiments, the plurality of openings opening(s) increase in size in order to increase conductance from the lid toward the bottom wall of the ampoule.

In one or more embodiments, the plurality of openings are notches located at a top end of the elongate walls near the lid. In one or more embodiments, each of the plurality of openings spans a longitudinal distance of greater than or equal to 1-5% to less than or equal to 100% of a length of the wall, including all values and subranges therebetween.

The degree of saturation of conventional ampoules decreases as the solid precursor is consumed due to an increase in volume of the precursor cavity. However, in the embodiments described, because sublimation occurs in the sublimation cavity, which is separated by filter media, the decrease of solid precursor does not affect the degree of saturation, as the volume of the sublimation cavity remains constant. Furthermore, in conventional ampoules, as the precursor is consumed, the gas flow is adjusted during processing to maintain sufficient ratios. However, in the embodiments described the gas flow can remain constant due to the constant volume of the sublimation cavity.

It is understood that the presence of inlet ports, outlet ports and channels/conduits is not limiting and that the number of ports, channels and conduits may be chosen based on space constraints and/or precursor characteristics and/or design need.

In some embodiments, the gas flow across the filter media and through the torturous path is sufficient to entrain and/or vaporize and/or sublime the precursor without a need for bubbling.

Thermocouples, mass flow meters, and pressure gauges may be included in the equipment denoted herein in order to monitor process conditions. In one or more embodiments, a mass flow meter is provided to monitor gas flow into the inlet port. In one or more embodiments, a thermocouple is installed in the bottom wall of the container and at any of the previously disclosed heater locations. In one or more embodiments, a pressure gauge is provided on the inlet line and/or the outlet line. A pressure range within the ampoule in accordance with some embodiments is greater than or equal to 25 torr to less than or equal to 150 torr.