Ampoule for semiconductor manufacturing precursors

Abstract

An ampoule for semiconductor manufacturing precursors and its method of use are described. The ampoule includes a container having an inlet port and an outlet port. The ampoule includes an inlet plenum located between the inlet port and a cavity, and an outlet plenum located between the outlet port and the cavity. A flow path is defined by a plurality of tubular walls and an entry opening in the ampoule, through which a carrier gas flows in contact with the precursor.

Description

[Technical field]

[0001] FIELD OF THE DISCLOSURE

[0001] This disclosure relates generally to ampoules for semiconductor manufacturing precursors and methods of using same. In particular, this disclosure relates to ampoules and methods that provide a tortuous flow path for low vapor pressure precursors. [Background technology]

[0002]

[0002] In the semiconductor industry, chemical vapor deposition (CVD) and atomic layer deposition (ALD) processes involve an increasing variety of chemicals that are provided in liquid or solid form. The precursors are typically contained in closed vessels or ampoules with a single inlet and a single outlet.

[0003]

[0003] Low vapor pressure precursors frequently use a carrier gas to carry the vapor from the ampoule to the process reactor. Two types of ampoules are commonly used in such processes: bubbler type, where the inlet carrier gas enters a tube immersed in the precursor, and cross-flow type, where the carrier gas sweeps out the headspace in the ampoule. In many cases, the carrier gas flow path is very short. The short flow path from the inlet to the outlet of the vessel does not allow sufficient residence time in the vessel for the carrier gas to become fully saturated with vaporized or sublimated precursor. Some existing ampoule designs do not distribute the carrier gas evenly across the surface of the precursor. Some existing ampoule designs do not adequately heat the precursor throughout the vessel. Many other solid source ampoules do not provide a means to prevent precursor dust from migrating downstream and degrading the performance of control valves or causing particle problems on the wafer.

[0004]

[0004] There is a need in the art for ampoules, particularly cross-flow ampoules, that have sufficient flow paths to saturate or nearly saturate the carrier gas with precursor and provide consistent delivery of the precursor, and methods of making and using the same. Summary of the Invention

[0005]

[0005] One or more embodiments are directed to an ampoule for semiconductor manufacturing precursors. The ampoule includes a container defining a cavity configured to hold a precursor. An inlet port and an outlet port are both in fluid communication with the cavity. The ampoule includes an inlet plenum located between the inlet port and the cavity, and an outlet plenum located between the outlet port and the cavity. A plurality of elongated walls contain the precursor and are arranged such that the walls define a flow channel. Each of the elongated walls includes an entry opening. A flow path is defined by the flow channel and the entry openings, through which a carrier gas flows in contact with the precursor.

[0006]

[0006] Additional embodiments of the present disclosure are directed to an ampoule for dispensing a vapor mixture of a carrier gas and a low vapor pressure precursor used in semiconductor manufacturing. The ampoule comprises a container having a bottom wall, a side wall, and a lid, the container defining a cavity configured to hold the precursor, such that a height (H) of the cavity extends from a lower surface of the lid to an upper surface of the bottom wall. A single inlet port and a single outlet port are both in fluid communication with the cavity. The ampoule includes an inlet plenum located between the inlet port and the cavity, and an outlet plenum located between the outlet port and the cavity. A plurality of elongated tubular walls containing the precursor arranged to define a flow channel, each of the elongated walls including an entry opening, the entry openings being offset such that one entry opening does not overlap another entry opening. A serpentine flow path defined by the flow channel and the entry openings, through which the carrier gas flows in contact with the precursor.

[0007]

[0007] A further embodiment of the present disclosure is directed to a method of providing a precursor flow. The method includes flowing a carrier gas through an inlet port and an inlet plenum of an ampoule having a low vapor pressure precursor therein. The carrier gas flow is directed into the ampoule through a flow path defined by a plurality of elongated walls and an entry opening in each of the elongated walls to contact the precursor. The carrier gas and precursor exit the ampoule via an outlet plenum and an outlet port.

[0008]

[0008] In order to be able to understand the above-mentioned features of the present invention in detail, a more detailed description of the present disclosure briefly summarized above can be obtained by referring to the embodiments. Some of the embodiments are shown in the accompanying drawings. However, it should be noted that the accompanying drawings only illustrate the typical embodiments of the present invention, and therefore should not be considered as limiting the scope of the present invention, since the present invention may also tolerate other equally effective embodiments. [Brief description of the drawings]

[0009] [Figure 1A] FIG. 1 shows a schematic diagram of an ampoule and associated manifold having an “outside-to-inside flow” configuration, according to one embodiment. [Figure 1B] FIG. 1 shows a schematic diagram of an ampoule and associated manifold having an “inside-to-outside flow” configuration according to another embodiment. [Diagram 2] 1B illustrates a cross-sectional view of FIG. 1A according to one or more embodiments. [Diagram 3] FIG. 3 shows a top perspective view of the tubular wall of the ampoule according to FIGS. 1A and 2 with flow annotations according to one or more embodiments. [Figure 4] 3 shows a perspective cross-sectional view of the ampule and a portion of the manifold of FIG. 2. [Diagram 5] 1 shows a schematic diagram of a bottom wall of an ampoule according to one embodiment. [Figure 6] FIG. 1C illustrates a perspective cross-sectional view of a portion of the ampoule and manifold of FIG. 1B according to one or more embodiments. [Figure 7] FIG. 7 shows a top perspective view of the tubular wall of the ampoule according to FIG. 1B and FIG. 6 with flow annotations according to one or more embodiments. [Figure 8] FIG. 1 illustrates a side perspective view of an exemplary tubular wall according to one or more embodiments. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0010]

[0018] In the accompanying drawings, similar components and / or features may have the same reference numbers. Additionally, various components of the same type may be distinguished by a dash after the reference number and a second number that distinguishes between the similar components. If only a first reference number is used in this specification, the description is applicable to any one of the similar components having the same first reference number, regardless of the second reference number. The cross-hatch shading of components in the figures is intended to aid in the visualization of different parts and does not necessarily indicate different material constructions.

[0011]

[0019] Before describing some example embodiments of the invention, it is to be understood that the invention is not limited to the details of construction or process steps set forth in the following description as the invention is capable of other embodiments and of being practiced or carried out in various ways.

[0012]

[0020] Some embodiments of the present disclosure advantageously provide a long flow path of carrier gas from the inlet to the outlet of the ampoule for the delivery of low vapor pressure precursors, e.g., liquid and / or solid source precursors. 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, more typically less than 1 Torr. In some applications, a carrier gas may be used to deliver low vapor pressure materials from the ampoule to the reactor. Materials with low vapor pressures typically require the application of 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 indium hafnium.

[0013]

[0021] A flow path having a long distance provides sufficient residence time for the carrier gas to go from being partially saturated to being nearly saturated or fully saturated with vaporized and / or sublimated and / or entrained precursors, the term "saturated" being used herein to allow for various degrees of saturation.

[0014]

[0022] Embodiments herein also provide methods for heating low vapor pressure precursors in large volume ampoules, including methods for providing effective uniform heating of the precursor. In some specific embodiments, low vapor pressure precursors, including solid precursor dust, are advantageously kept within the vessel cavity and prevented from migrating upstream or downstream of the control valve. Some embodiments advantageously control uneven depletion of the precursor. Some embodiments advantageously provide uniform distribution of carrier gas along the entire surface of the precursor. Embodiments herein provide improved dosage of precursor. The designs provided herein can provide high volume ampoules with a smaller footprint than other designs. The designs herein are easy to clean and refill. The designs herein can accommodate precursor charges up to 10-20 kilograms.

[0015]

[0023] In some embodiments, the ampoule includes a plurality of elongated walls that define a serpentine labyrinth of flow paths. Advantageously, one or more embodiments provide flow paths that can be 5-10 times longer than those found in typical ampoules, particularly solid source sublimation vessels.

[0016]

[0024] The ampoule comprises a container defining a cavity configured to hold a precursor, an inlet port and an outlet port, both in fluid communication with the cavity, an inlet plenum and an outlet plenum, each located between the inlet port or outlet port and the cavity, and a plurality of elongated walls, each of which defines an entry opening, containing the precursor arranged to define a flow channel. The flow channel is defined by the flow channel and the entry opening, through which a carrier gas flows in contact with the precursor. In one or more embodiments, the flow path moves from the outermost channel to the innermost channel, which may be referred to as an "outside-to-inside flow" configuration. In one or more embodiments, the flow path moves from the innermost channel to the outermost channel, which may be referred to as an "inside-to-outside flow" configuration.

[0017]

[0025] In general, the flow paths provided herein force the carrier gas to flow around a series of elongated walls, which in one or more specific embodiments are nested concentric tubes that define a flow channel, each containing a volume of solid precursor. The gas flow changes direction from flow channel to flow channel until it reaches the last flow channel that communicates with an outlet port. This change in direction promotes mixing of the vaporized and / or sublimated precursor with the carrier gas. The entry openings allow the carrier gas to flow into the next flow channel. References herein to gas flow include carrier gas alone or in combination with entrained and / or vaporized and / or sublimated precursor. It is understood that the flow paths described herein, for example with respect to FIG. 3 or FIG. 6, are a series of elongated walls, tubes or the like with entry openings configured to define flow channels therebetween to provide the desired flow path. Preferably, the entry openings are offset so that the flow channels are not bypassed.

[0018]

[0026] 1A is a schematic diagram of an ampoule and associated manifold having an "outside-to-in flow" configuration according to an embodiment. Ampoule 100 and manifold 102 are suitable for use with semiconductor manufacturing materials including reagents and precursors. The term "precursor" is used to describe the contents of ampoule 100 and refers to any reagent that flows into the process environment.

[0019]

[0027] The ampoule 100 includes a vessel 110 having a bottom wall 112, a side wall 114, and a lid 116. An inlet port 120 and an outlet port 130 are in fluid communication with a cavity defined by the interior walls of the vessel 110. The inlet port 120 is generally configured to allow connection to a gas source "G" by suitable tubing and valve(s) and may have a suitable threaded or sealed connection. In one or more embodiments, the gas source "G" is a carrier gas, which in one or more embodiments is inert. The outlet port 130 is also in fluid communication with the cavity. The outlet port 130 is generally configured to allow connection to a line including suitable tubing and valve(s) to allow a flow of gas, which may include entrained particles, to flow out of the vessel 110 and into a processing chamber (or other component) "P". The outlet port 130 may have a welded or threaded connection to allow a gas line to be connected.

[0020]

[0028] The height (H) of the cavity defined by the container 110 extends from the lower surface of the lid 116 to the upper surface of the bottom wall 112 .

[0021]

[0029] Turning to the embodiment of Figure 2, which shows the cross-section of Figure 1A, the ampoule includes a single inlet port 120 and a single outlet port 130. Although the embodiment of Figure 2 depicts one inlet port and one outlet port, there may be multiple inlet and outlet ports if required by a particular application. The positions of the inlets and outlets may be interchanged to accommodate other designs.

[0022]

[0030] FIG. 4 shows a perspective cross-sectional view of a portion of the ampoule and manifold of FIG. 2, and FIG. 5 shows a schematic diagram of the bottom wall of the ampoule in one embodiment.

[0023]

[0031] 2 and 4, the inlet port 120 has a passageway 121 that extends partially through the depth of the lid 116 and has an inner diameter that defines a cross-sectional width of the passageway 121. The passageway 121 is in fluid communication with the inlet port plenum 122. The inlet port plenum 122 is designed to accommodate a volume of incoming carrier gas from a source "G" which then flows into a cavity generally designated 118. The inlet port plenum 122 is sized to not restrict the flow of the incoming carrier gas. The inlet port plenum 122 may be positioned and / or sized to accommodate an incoming flow line.

[0024]

[0032] The outlet port 130 has a passageway 131 having an inner diameter that defines a cross-sectional width of the passageway 131 that extends partially through the depth of the lid 116. The passageway 131 is in fluid communication with an outlet port plenum 132. The outlet port plenum 132 is designed to accommodate a volume of entrained and / or saturated exiting carrier gas that then exits the ampoule downstream into the processing chamber "P". The outlet port plenum 132 is sized to not restrict the flow of the entrained and / or saturated exiting carrier gas. The outlet port plenum 132 may be positioned and / or sized to accommodate the exiting flow lines.

[0025]

[0033] Specifically with respect to this embodiment, cavity 118 is comprised of a number of flow channels 124a-124e defined by a number of elongated walls 126a-126d. Each of elongated walls 126a-126d includes an entry opening, such as entry opening 128a in wall 126a, entry opening 128b in wall 126b, entry opening 128c in wall 126c, and entry opening 128d in wall 126d. The entry openings are offset such that one entry opening does not overlap another entry opening.

[0026]

[0034] 2 and 4-5, in this embodiment, the plurality of elongated walls 126a-126d at the bottom edge or rim reside in or fit with corresponding grooves 113a-113d in the upper surface of the bottom wall 112. The lower surface of the lid 116 optionally includes a plurality of grooves 117a-117d. In one or more embodiments, in the absence of a distribution element 134, the plurality of elongated walls 126a-126d at the top edge or rim may reside in or fit with corresponding grooves 117a-117d. The elongated walls 126a-126d extend to the bottom wall 116 and extend towards the lid 112, optionally to the height of a cavity extending into the lid 112. The elongated walls are effective to conduct heat from one or more external sources.

[0027]

[0035] There is optionally a distribution element 134 sandwiched between the lid and the top edge of the elongated wall. The distribution element 134 is disposed between the cavity 118 and both the inlet plenum 122 and the outlet plenum 132. That is, flow exiting the inlet plenum 122 passes through the distribution element 134 before entering the cavity 118, and flow exiting the cavity 118 passes through the distribution element 134 before entering the outlet plenum 132.

[0028]

[0036] The distribution element can be of any suitable material or configuration or size or media grade that provides one or more of the following characteristics: withstands long term exposure to precursor, does not induce a pressure drop that would prevent effective delivery of precursor, pore size that inhibits and / or prevents precursor particulates and / or droplets from exiting the ampoule to protect both the inlet and outlet devices, and flexibility that allows for a slight seal between the end of the elongated wall and the inner diameter of the cavity. In one or more embodiments, the distribution element is a porous disk of filter media. In one or more embodiments, the distribution element is a sintered porous stainless steel material. Non-limiting exemplary porosity of the distribution element can be from 0.1 μm or more to less than 100 μm, and all values ​​and subranges therebetween, as measured by the average pore size.

[0029]

[0037] Additionally, there is optionally a shim between the lower surface of the distribution element and the upper edge of the elongated wall, which is described in more detail with respect to shim 236 in FIG.

[0030]

[0038] In some embodiments, ampoule 100 includes a low vapor pressure material 150 in cavity 118 that resides in a flow channel defined by elongated walls 126a-126d. The space above the material in cavity 118 and below the underside of the lid is referred to as the headspace of ampoule 100. Dispensing element 134, if present, is disposed in the headspace within the ampoule. Material 150 may be a precursor for use in a semiconductor manufacturing process. In one or more embodiments, the low vapor pressure material is a solid.

[0031]

[0039] 2, the lid 116 is a separate component from the bottom wall 112 and the side wall 114. The lid 116 can be connected to the side wall 114 of the vessel 110 with a removable bolt through an appropriately shaped opening, and may have threads to facilitate connection of a threaded bolt. By removing the bolt, the lid 116 can be removed from the vessel 110 to change or add precursor 150 within the vessel 110.

[0032]

[0040] The lid may further include one or more exterior surface features for interfacing with an external heater. The bottom wall may be configured for interfacing with an external heater. One or more jacket heaters may be provided around the side walls.

[0033]

[0041] A first seal 152 is positioned between an upper surface of the sidewall 114 and a lower surface of the lid 116 to form a fluid-tight seal. A second seal 154 is positioned between an upper portion of the bottom wall 112 and a lower surface of the sidewall 114 to form a fluid-tight seal. In some embodiments, the first seal 152 and the second seal 154 are separate O-rings.

[0034]

[0042] In some embodiments (not shown), the lid 116 may be integrally formed with the side wall 114 and bottom wall 112 of the container 110 .

[0035]

[0043] Different manifold configurations can be connected to the lid 116 to allow for the addition of the ampoule 100 to the processing chamber. In some embodiments, an inlet line 170 is connected to the inlet port 120. An inlet valve 172 can be disposed on the inlet line 170 between the gas source "G" and the inlet port 120. The inlet valve 172 can be integrally formed with the lid 116 or can be connected to the lid 116 as a separate component. An outlet line 180 can be connected to the outlet port 130. The outlet line 180 in some embodiments includes an outlet valve 182 located between the outlet port 130 and the processing chamber "P". The inlet valve 172 and the outlet valve 182 can be used to isolate the ampoule 100 such that the contents of the cavity 118 are isolated from the environment outside the container 110. In some embodiments, there are multiple valves along the inlet line 170 (e.g., 174) and / or the outlet line 180 (e.g., 184) and / or in between (e.g., 190). The valves can be manual valves or pneumatic valves.

[0036]

[0044] FIG. 3 shows a top perspective view of elongated walls 126a-d of an ampoule with flow annotations according to one or more embodiments. In one or more embodiments, elongated walls 126a-d include elongated tubular walls that define a series of flow channels 124a-e. As depicted in FIG. 3, in one or more embodiments, elongated walls 126a-d are concentric tubular. The relative position of the walls can be adjusted, for example, to favor precursor reduction in a desired matter. In one or more embodiments, the annular distance between the walls varies. The use of tubular elongated walls made by nesting readily available tubes can ease assembly and reduce the cost of the ampule.

[0037]

[0045] A carrier gas flow enters the ampoule 100 from the inlet port 120 via the inlet plenum 122 as described with respect to FIG. 2. The carrier gas enters the flow channel 124a defined by the sidewall 114 (shown in FIG. 4) and the elongated wall 126a and contacts the precursor 150, thereby entraining and / or vaporizing the precursor as the carrier gas passes over the surface of the precursor volume. The flow then proceeds through the entrance opening 128a in the elongated wall 126a, at which point the carrier gas enters the flow channel 124b, and the surface of the elongated wall 126b opposite the entrance opening 128a directs the flow through the flow channel 124b in two directions depicted by the arrows B1 and B2. While in the flow channel 124b, the carrier gas continues to contact and become saturated with the precursor 150. Similarly, the flow then proceeds through entrance opening 128b in elongated wall 126b, at which point the carrier gas enters flow channel 124c, the surfaces of which direct the flow in two directions depicted by arrows C1 and C2 through flow channel 124c. While in flow channel 124c, the carrier gas continues to contact and becomes saturated with precursor 150. Similarly, the flow then proceeds through entrance opening 128c in elongated wall 126c, at which point the carrier gas enters flow channel 124d, the surfaces of which direct the flow in two directions depicted by arrows D1 and D2 through flow channel 124d. While in flow channel 124d, the carrier gas continues to contact and becomes saturated with precursor 150. Finally, the flow proceeds through entry opening 128d in elongated wall 126d, at which point the carrier gas enters flow channel 124e, depicted by arrows E1 and E2, and exits the ampoule through outlet plenum 132 and outlet port 130. While in flow channel 124e, the carrier gas continues to contact and become saturated with precursor 150.

[0038]

[0046] Thus, the flow channels 124a-124e are nested to include a plurality of serpentine passages (124a, 124b, 124c, 124d) and an outlet passage (124e) such that, with respect to the serpentine passages, flow through the first entry openings (128a, 128b, 128c) diverts the carrier gas to first and second portions that flow in first and second directions (e.g., B1 and B2, C1 and C2, and D1 and D2) through first and second sections, respectively, of the serpentine passages.

[0039]

[0047] 1B shows a schematic diagram of an ampoule and associated manifold having an "inside-to-out flow" configuration according to an embodiment. Ampoule 200 and manifold 202 are suitable for use with semiconductor manufacturing materials including reagents and precursors. The term "precursor" is used to describe the contents of ampoule 200 and refers to any reagent that flows into a processing environment.

[0040]

[0048] The ampoule 200 includes a vessel 210 having a bottom wall 212, a side wall 214, and a lid 216. An inlet port 220 and an outlet port 230 are in fluid communication with a cavity defined by the interior walls of the vessel 210. The inlet port 220 is generally configured to allow connection to a gas source "G" by suitable tubing and valve(s) and may have a suitable threaded or sealed connection. In one or more embodiments, the gas source "G" is a carrier gas, which in one or more embodiments is inert. The outlet port 230 is also in fluid communication with the cavity. The outlet port 230 is generally configured to allow connection to a line including suitable tubing and valve(s) to allow a flow of gas, which may include entrained particles, to flow out of the vessel 210 and into a processing chamber (or other component) "P". The outlet port 230 may have a welded or threaded connection to allow a gas line to be connected.

[0041]

[0049] The height (H) of the cavity defined by the container 210 extends from the lower surface of the lid 216 to the upper surface of the bottom wall 212 .

[0042]

[0050] Turning to the embodiment of Figure 6, which shows a perspective cross-section of the ampoule and a portion of the manifold of Figure 1B, the ampoule includes a single inlet port 220 and a single outlet port 230. Although the embodiment of Figure 6 depicts one inlet port and one outlet port, there may be multiple inlet and outlet ports if a particular application requires. The positions of the inlets and outlets may be interchanged to accommodate other designs.

[0043]

[0051] 6, the inlet port 220 has a passageway 221 that extends partially through the depth of the lid 116 and has an inner diameter that defines a cross-sectional width of the passageway 221. The passageway 121 is in fluid communication with the inlet port plenum 222. The inlet port plenum 222 is designed to accommodate a volume of incoming carrier gas from a source "G" which then flows into a cavity generally shown as 218. The inlet port plenum 222 is sized to not restrict the flow of the incoming carrier gas. The inlet port plenum 222 may be positioned and / or sized to accommodate an incoming flow line.

[0044]

[0052] The outlet port 230 has a passageway 231 having an inner diameter that defines a cross-sectional width of the passageway 231 that extends partially through the depth of the lid 216. The passageway 231 is in fluid communication with an outlet port plenum 232. The outlet port plenum 232 is designed to accommodate a volume of entrained and / or saturated exiting carrier gas that then exits the ampoule downstream into the processing chamber "P". The outlet port plenum 232 is sized to not restrict the flow of the entrained and / or saturated exiting carrier gas. The outlet port plenum 232 may be positioned and / or sized to accommodate the exiting flow lines.

[0045]

[0053] Specifically with respect to this embodiment, cavity 218 is comprised of a plurality of flow channels 224a-224e defined by a plurality of elongated walls 226a-226d. Each of elongated walls 226a-226d includes an entry opening, such as entry opening 228a in wall 226a, entry opening 228b in wall 226b, entry opening 228c in wall 226c, and entry opening 228d in wall 226d. The entry openings are offset such that one entry opening does not overlap another entry opening.

[0046]

[0054] In one or more embodiments, a number of elongated walls 226a-226d at the bottom edge or rim may be present or mate with corresponding grooves (not shown in FIG. 6 but similar to 113a-113d) in the upper surface of the bottom wall 212. In this embodiment, the underside of the lid 216 is devoid of grooves. The elongated walls 226a-226d extend into the bottom wall 216 and widen towards the lid 212 the height of the cavity. The elongated walls are effective to conduct heat from one or more external sources.

[0047]

[0055] 2 and 4, is optionally sandwiched between the lid and the upper edge of the elongated wall. The distribution element 234 is disposed between the cavity 218 and both the inlet plenum 222 and the outlet plenum 232. That is, flow exiting the inlet plenum 222 passes through the distribution element 234 before entering the cavity 218, and flow exiting the cavity 218 passes through the distribution element 234 before entering the outlet plenum 232.

[0048]

[0056] In the embodiment of Figure 6, a shim 236 is placed between the lower surface of the distribution element and the upper edge of the elongated wall. The shim has openings corresponding to the flow channels 224a and 224e to allow unrestricted flow. The shim is a soft, compliant material, for example, a soft metal such as aluminum or a flexible polymeric or elastomeric material. The shim provides support to the distribution element 234.

[0049]

[0057] In some embodiments, ampoule 200 includes a low vapor pressure material in cavity 218 that resides in a flow channel defined by elongated walls 226a-226d. The space above the material in cavity 218 and below the underside of the lid is referred to as the headspace of ampoule 200. Dispensing element 234, if present, is disposed in the headspace within the ampoule. The material may be a precursor for use in a semiconductor manufacturing process. In one or more embodiments, the low vapor pressure material is a solid.

[0050]

[0058] In some embodiments, as shown in Figure 6, the lid 216 is a separate component from the bottom wall (e.g., 212 in Figure 1A) and side wall 214. The lid 216 can be connected to the side wall 214 of the vessel with a removable bolt through an appropriately shaped opening, and may have threads to facilitate connection of a threaded bolt. The bolts can be removed to remove the lid 216 from the vessel so that the precursors in the vessel can be changed or added.

[0051]

[0059] The lid may further include one or more exterior surface features for interfacing with an external heater. The bottom wall may be configured for interfacing with an external heater. One or more jacket heaters may be provided around the side walls.

[0052]

[0060] A first seal 252 is located between the upper surface of the sidewall 214 and the lower surface of the lid 216 to form a fluid-tight seal. A second seal is disposed between the top of the bottom wall and the lower surface of the sidewall to form a fluid-tight seal. In some embodiments, the first seal 252 and the second seal are separate O-rings.

[0053]

[0061] In some embodiments (not shown), the lid 216 may be integrally formed with the sidewalls 214 and bottom wall of the container.

[0054]

[0062] As discussed with respect to FIG. 2, different manifold configurations can be connected to the lid 216 to allow for the addition of ampoules 200 to the processing chamber.

[0055]

[0063] FIG. 7 shows a top perspective view of elongated walls 226a-d of an ampoule with flow annotations according to one or more embodiments. In one or more embodiments, elongated walls 226a-d include elongated tubular walls that define a series of flow channels 224a-e. As depicted in FIG. 7, in one or more embodiments, elongated walls 226a-d are concentric tubular. The relative positions of the walls can be adjusted to favor, for example, precursor reduction in a desired material. In one or more embodiments, the annular distance between the walls varies. The use of tubular elongated walls made by nesting readily available tubes can ease assembly and reduce the cost of the ampule.

[0056]

[0064] A carrier gas flow enters the ampoule 200 from the inlet port 220 via the inlet plenum 222, as described with respect to FIG. 6. The carrier gas enters the flow channel 224e defined by the elongated wall 226d and contacts the precursors, thereby entraining and / or vaporizing the precursors as the carrier gas passes over the surface of the precursor volume. The flow then proceeds through the entrance opening 228d in the elongated wall 226d, at which point the carrier gas enters the flow channel 224d, and the surface of the elongated wall 226c opposite the entrance opening 228d directs the flow through the flow channel 224d in the two directions depicted by the arrows F1 and F2. While in the flow channel 224d, the carrier gas continues to contact the precursors and becomes saturated. Similarly, the flow then proceeds through entrance opening 228c in elongated wall 226c, at which point the carrier gas enters flow channel 224c, and the surface of elongated wall 226b directs the flow in two directions depicted by arrows G1 and G2 through flow channel 224c. While in flow channel 224c, the carrier gas continues to contact and become saturated with the precursors. Similarly, the flow then proceeds through entrance opening 228b in elongated wall 226b, at which point the carrier gas enters flow channel 224b, and the surface of elongated wall 226a directs the flow in two directions depicted by arrows H1 and H2 through flow channel 224b. While in flow channel 224b, the carrier gas continues to contact and become saturated with the precursors. Finally, the flow then proceeds through entry opening 228a in elongated wall 226a, at which point the carrier gas enters flow channel 224a, depicted by arrows I1 and I2, defined by sidewall 214 (shown in FIG. 6) and elongated wall 226a, and exits the ampoule through outlet plenum 132 and outlet port 130. While in flow channel 224a, the carrier gas continues to contact and become saturated with the precursor.

[0057]

[0065] Thus, flow channels 224a-224e are nested including a plurality of serpentine passages (224e, 224d, 224c, 224b) and an outlet passage (224a), and with respect to the serpentine passages, flow through first entry openings (228d, 228c, 228b) diverts carrier gas in first and second directions (e.g., F1 and F2, G1 and G2, H1 and H2) through first and second sections of the serpentine passage, respectively.

[0058]

[0066] According to one or more embodiments, the entry openings of any embodiment are suitable for allowing the flow of carrier gas from one flow channel to another. The entry openings can be of any suitable shape and / or configuration and / or location to accommodate the flow of entrained and / or saturated carrier gas along the elongated wall. The entry openings can span the entire length of the container or can vary in length. The entry opening features can be multiple holes, tapered slots, or other shapes. In one or more embodiments, the entry openings are sized and shaped to vary the conductance of the carrier gas along the longitudinal distance of the container. In one or more examples, the size of the entry opening(s) is increased to increase the conductance from the lid to the bottom wall of the ampoule. FIG. 8 is a side perspective view of an exemplary tubular wall 326 that includes a wedge-shaped entry opening 328 that progresses along the length of the elongated wall and increases in size from the lid edge 330 to the bottom wall edge 332, enhancing conductance from the lid toward the bottom wall of the ampoule.

[0059]

[0067] In one or more embodiments, the access openings are notches located at the upper ends of the elongated walls near the lid, In one or more embodiments, each of the access openings extends a longitudinal distance of from 1-5% or more to 100% or less of the length of the wall, including all values ​​and sub-ranges therebetween.

[0060]

[0068] In one or more embodiments, the access openings are a plurality of holes in each wall spaced apart along the length of each wall, hi one or more embodiments, the plurality of holes spaced apart along the length of each wall increase in size from the lid edge to the bottom wall edge.

[0061]

[0069] According to one or more embodiments, when the ampoule contains a minimum amount of precursor, the carrier gas is expected to be fully saturated over the flow path distance, which may depend on the particular precursor in the ampoule and its physical properties. As the amount of precursor level in the ampoule decreases during use, the degree of saturation may decrease. Saturation may vary as a function of fill level.

[0062]

[0070] It is understood that the presence of five flow channels in Figures 2-3 is not limiting and the number of channels may be selected based on space constraints and / or precursor properties and / or design needs.

[0063]

[0071] In some embodiments, the gas flow through the inlet port 120 and along the flow path is sufficient to entrain and / or vaporize and / or sublimate the precursor without the need for bubbling. The gas flow can be adjusted during processing as the precursor 150 level decreases to maintain sufficient contact. The gas flow in some embodiments has a maximum velocity in combination with a heat source sufficient to prevent condensation of the precursor 150 at the outlet port 130.

[0064]

[0072] Thermocouples, mass flow meters, and pressure gauges may be included in the instruments shown herein to monitor process conditions. In one or more embodiments, a mass flow meter is provided to monitor gas flow to the inlet port. In one or more embodiments, a thermocouple is installed in the lid. In one or more embodiments, a pressure gauge is provided on the inlet line and / or the outlet line. The pressure range in the ampoule according to some embodiments is from 25 torr or more to 150 torr or less.

[0065]

[0073] References throughout this specification to "one embodiment," "certain embodiments," "one or more embodiments," or "an embodiment" mean that a particular feature, structure, material, or characteristic described in connection with that embodiment is included in at least one embodiment of the invention. Thus, the appearances of phrases such as "in one or more embodiments," "in certain embodiments," or "in an embodiment" in various places throughout this specification do not necessarily refer to the same embodiment of the invention. Furthermore, the particular features, structures, materials, or characteristics may be combined in any suitable manner in one or more embodiments.

[0066]

[0074] Although the present invention has been described with reference to particular embodiments, it should be understood that these embodiments are merely illustrative of the principles and applications of the present invention. It will be apparent to those skilled in the art that various modifications and variations can be made to the method and apparatus of the present invention without departing from the spirit and scope of the invention. Thus, it is intended that the present invention cover such modifications and variations as come within the scope of the appended claims and their equivalents.

Claims

1. 1. An ampoule for semiconductor manufacturing precursors, comprising: a container defining a cavity configured to hold the precursor; an inlet port having a passage extending through the depth of the vessel and an outlet port having a passage extending through the depth of the vessel, both in fluid communication with the cavity; an inlet plenum located between the inlet port and the cavity; an outlet plenum located between the outlet port and the cavity; a plurality of elongated walls arranged to define a flow channel containing the precursor, each of the elongated walls including an entry opening; a flow path defined by the flow channel and the entry opening, through which a carrier gas flows in contact with the precursor; wherein each of the entry openings progresses along a length of the elongated wall such that an opening size increases from a lid edge to a bottom wall edge of the elongated wall.

2. 10. The ampoule of claim 1, wherein the plurality of elongated walls and the access opening define a labyrinth such that the flow path is serpentine.

3. 10. The ampoule of claim 1, wherein the entry openings are offset such that one entry opening does not overlap another entry opening.

4. 10. The ampoule of claim 1, wherein the ampoule comprises a single inlet and a single outlet.

5. The ampoule of claim 1 , further comprising a distribution element located between the cavity and both the inlet and outlet plenums.

6. The ampoule of claim 1 , wherein each of the entry openings is wedge-shaped.

7. 10. The ampoule of claim 1, wherein the plurality of elongated walls are effective to conduct heat from an external heat source.

8. 2. The ampoule of claim 1, wherein the flow channel is nested, the flow channel comprising a plurality of serpentine paths and an outlet path, such that, for the serpentine paths, flow through a first entry opening diverts the carrier gas to first and second portions that flow in first and second directions, respectively, through first and second sections of the serpentine path.

9. 1. An ampoule for dispensing a vapor mixture of a carrier gas and a low vapor pressure precursor for use in semiconductor manufacturing, comprising: a container having a bottom wall, a side wall, and a lid, the container defining a cavity configured to hold the precursor, such that a height (H) of the cavity extends from a lower surface of the lid to an upper surface of the bottom wall; a single inlet port having a passageway extending a portion of the depth of the lid and a single outlet port having a passageway extending a portion of the depth of the lid, both in fluid communication with the cavity; an inlet plenum located between the inlet port and the cavity; an outlet plenum located between the outlet port and the cavity; a plurality of elongated tubular walls containing the precursor and arranged to define a flow channel, each of the elongated tubular walls including an entry opening, the entry openings being offset such that one entry opening does not overlap another entry opening; a serpentine flow path defined by the flow channel and the entry opening, through which a carrier gas flows in contact with the precursor; wherein each of the entry openings progresses along a length of the elongated tubular wall such that the opening size increases from a lid edge to a bottom wall edge of the elongated tubular wall.

10. 10. The ampoule of claim 9, including a distribution element positioned between the cavity and both the inlet plenum and the outlet plenum and extending a distance of at least an inner diameter defined by the sidewall.

11. 10. The ampoule of claim 9, wherein each of the entry openings is wedge-shaped.

12. 10. The ampoule of claim 9, wherein said plurality of elongated tubular walls are concentric.

13. 10. The ampoule of claim 9, wherein the bottom wall includes a plurality of grooves that mate with the plurality of elongated tubular walls.

14. 10. The ampoule of claim 9, wherein the length of the flow path is effective to saturate the carrier gas with the precursor.

15. 10. The ampoule of claim 9, wherein the plurality of elongated tubular walls are effective to conduct heat from an external heat source.

16. 10. The ampoule of claim 9, wherein the flow channel is nested, the flow channel comprising a plurality of serpentine paths and an outlet path, such that, for the serpentine paths, flow through a first entry opening diverts the carrier gas to first and second portions that flow in first and second directions, respectively, through first and second sections of the serpentine path.

17. 1. A method for providing a flow of precursor from an ampoule having a low vapor pressure precursor therein, comprising: flowing a carrier gas through an inlet port having a passageway extending through the depth of the ampoule and through an inlet plenum of the ampoule; directing the flow of the carrier gas within the ampoule through a flow passage defined by a plurality of elongated walls and an entry opening in each of the elongated walls such that the carrier gas flows in contact with the precursor; flowing the carrier gas and the precursor out of the ampoule through an outlet plenum and an outlet port having a passageway extending through the depth of the ampoule; wherein each of the entry openings progresses along a length of the elongated wall such that an opening size increases from a lid edge to a bottom wall edge of the elongated wall.

18. The method of claim 17 , wherein the length of the flow path is effective to saturate the carrier gas with the precursor.

19. 20. The method of claim 17, further comprising independently heating a lid and a bottom wall of the ampoule, the plurality of elongated walls being effective to conduct heat from an external heat source.

20. 18. The method of claim 17, wherein the flow path includes nested passages such that flow through a first entry opening diverts the carrier gas to first and second portions, the first and second portions respectively flowing in first and second directions through first and second sections of the nested passages.

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