Ampoule for semiconductor manufacturing precursor

Abstract

To provide a cross-flow ampoule for a semiconductor manufacturing precursor having a flow path sufficient to saturate a carrier gas with the precursor and provide consistent delivery of the precursor, and a method of providing a flow of the precursor.SOLUTION: The ampoule includes a container having an inlet port 120 and an outlet port 130. The ampoule comprises an inlet plenum 122 located between the inlet port and the cavity 118 and an outlet plenum 132 located between the outlet port and the cavity. A flow path is defined by the plurality of tubular walls 126a to 126d and the entry opening 128a to 128d of the ampule through which the carrier-gas flows in contact with the precursor.SELECTED DRAWING: Figure 2

Description

Technical Field

[0001]

[0001] This disclosure generally relates to ampoules for semiconductor manufacturing precursors and methods of using the same. Specifically, this disclosure relates to ampoules and methods that provide a serpentine flow path for low vapor pressure precursors.

Background Art

[0002]

[0002] In the semiconductor industry, the types of chemicals provided in liquid or solid form are increasing in chemical vapor deposition (CVD) and atomic layer deposition (ALD) processes. Precursors are typically in a closed container, an ampoule, having a single inlet and a single outlet.

[0003]

[0003] Low vapor pressure precursors frequently use a carrier gas to transport vapor from the ampoule to the processing reactor. In such processes, generally two types of ampoules are used. There are the bubbler type where the inlet carrier gas enters a tube immersed in the precursor, and the cross-flow type ampoule where the carrier gas sweeps the headspace inside the ampoule. In many cases, the flow path of the carrier gas is very short. Since the flow path from the inlet to the outlet of the container is short, sufficient residence time inside the container cannot be ensured until the carrier gas is completely saturated with the vaporized or sublimated precursor. Among existing ampoule designs, there are those where the carrier gas does not uniformly spread over the entire surface of the precursor. Among existing ampoule designs, there are also those that cannot sufficiently heat the precursor throughout the container. Many other solid source ampoules do not have means to prevent the precursor dust from moving downstream and degrading the performance of the control valve or causing particle problems on the wafer.

[0004]

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

Summary of the Invention

[0005]

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

[0007]

[0007] Further embodiments of the present disclosure are directed to a method of providing a flow of a precursor. 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 flow of the carrier gas is directed into the ampoule through a flow path defined by a plurality of elongated walls and an inlet opening of each of the elongated walls and contacts the precursor. The carrier gas and the precursor flow out of the ampoule through an outlet plenum and an outlet port.

[0008]

[0008] To enable a more detailed understanding of the above-described features of the present invention, a more detailed description of the present disclosure, briefly summarized above, can be obtained by reference to the embodiments. Some of the embodiments are illustrated in the accompanying drawings. However, it should be noted that the accompanying drawings illustrate only typical embodiments of the present invention and, therefore, should not be regarded as limiting the scope of the present invention since the present invention may admit other equally effective embodiments.

Brief Description of the Drawings

[0009]

Figure 1A

Figure 1B

Figure 2

Figure 3

Figure 4

Figure 5

Figure 6

Figure 7

Figure 8

[0010]

[0018] In the accompanying drawings, similar components and / or features may have the same reference numerals. Further, various components of the same type may be distinguished by appending a dash after the reference numeral and a second numeral that differentiates between similar components. When only the first reference numeral is used herein, the description is applicable to any one of the similar components having the same first reference numeral, regardless of the second reference numeral. The cross-hatching density of the components in the figures is for assisting in visualizing different parts and does not necessarily indicate different material structures.

[0011]

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

[0012]

[0020] Some embodiments of the present disclosure advantageously provide a long flow path for a carrier gas from an inlet to an outlet of an ampoule for delivery of a low vapor pressure precursor, e.g., a liquid and / or solid source precursor. A low vapor pressure precursor is understood to refer to a material that does not readily vaporize under atmospheric conditions. A low vapor pressure precursor typically has a vapor pressure of less than 10 Torr, more typically less than 1 Torr. Depending on the application, a carrier gas may be used to transport a low vapor pressure material from an ampoule to a reactor. Materials with low vapor pressures usually need to be heated to increase their 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 the carrier gas with sufficient residence time to go from a partially saturated state to a nearly saturated or fully saturated state by the vaporized and / or sublimated and / or entrained precursor. As used herein, the expression "saturated" allows for varying degrees of saturation.

[0014]

[0022] Embodiments herein also provide a method of heating a low vapor pressure precursor in a large volume ampoule, including a method of providing effective uniform heating of the precursor. In some specific embodiments, a low vapor pressure precursor including solid precursor dust is advantageously held within a cavity of a container and not moved upstream or downstream of a control valve. Some embodiments advantageously control a non-uniform decrease of the precursor. Some embodiments advantageously provide a uniform distribution of the carrier gas along the entire surface of the precursor. Embodiments herein provide an improved dosage of the precursor. The designs provided herein can provide a high-capacity (volume) ampoule with a smaller ground area than other designs. The designs herein are easy to clean and refill. The designs herein can accommodate precursor charges of up to 10 - 20 kilograms.

[0015]

[0023] In some embodiments, the ampoule includes a plurality of elongated walls that define a maze such that the flow path meanders. Advantageously, one or more embodiments provide a flow path whose distance can be 5 to 10 times longer than the distances found in typical ampoules, particularly solid source sublimation vessels.

[0016]

[0024] The ampoule includes a container that defines 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 the outlet port and the cavity, and a plurality of elongated walls including a precursor arranged to define a flow channel, each of which constitutes an inlet opening. The flow path is defined by the flow channel and the inlet opening, through which the 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 "outer-to-inner 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 "inner-to-outer flow" configuration.

[0017]

[0025] Generally, the flow channels provided herein force a carrier gas to flow around a series of elongated walls. This wall is, in one or more particular embodiments, a concentric tube nested to 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 the outlet port. This change in direction promotes the mixing of the vaporized and / or sublimed precursor and the carrier gas. The inlet opening allows the carrier gas to flow into the next flow channel. References herein to gas flow include the carrier gas alone or in combination with entrained droplets and / or vaporized and / or sublimed precursors. It is understood that the flow channels described herein, for example, with respect to FIGS. 3 or 6, result in a desired flow channel with a series of elongated walls, tubes, or others configured to define the flow channels therebetween. Preferably, the inlet opening is offset so that the flow channel is not bypassed.

[0018]

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

[0019]

[0027] Ampoule 100 includes a container 110 having a bottom wall 112, side walls 114, and a lid 116. An inlet port 120 and an outlet port 130 are in fluid communication with a cavity defined by the inner wall of the container 110. The inlet port 120 is generally configured to enable connection to a gas source "G" by appropriate piping and valves (if any), and can have an appropriate threaded or sealed connection. In one or more embodiments, the gas source "G" is a carrier gas, and in one or more embodiments, the carrier gas is inert. Also, the outlet port 130 is in fluid communication with the cavity. The outlet port 130 is generally configured to be connectable to a line including appropriate piping and valves (if any) to direct a gas flow containing entrained particles out of the container 110 to a processing chamber (or other component) "P". The outlet port 130 may have a welded connection or a threaded connection to enable connection of a gas line.

[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 FIG. 2 which shows a cross-sectional view of FIG. 1A, the ampoule includes a single inlet port 120 and a single outlet port 130. In the embodiment of FIG. 2, one inlet port and one outlet port are depicted each, but multiple inlet ports and outlet ports may be present if required for a particular application. It is also possible to adapt to other designs by swapping the positions of the inlet and outlet.

[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 view of the bottom wall of an ampoule of one embodiment.

[0023]

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

[0024]

[0032] The outlet port 130 has a passage 131 that extends into a portion of the lid 116 in the depth direction and has an inner diameter that defines the cross-sectional width of the passage 131. The passage 131 is in fluid communication with the outlet port plenum 132. The outlet port plenum 132 is designed to accommodate the volume of the carrier gas that is entrained and / or saturated and flows out, and this carrier gas then flows out from the ampoule into the downstream processing chamber "P". The outlet port plenum 132 is sized such that it does not restrict the flow of the carrier gas that is entrained and / or saturated and flows out. The outlet port plenum 132 may be positioned and / or sized to accommodate the outflow flow line.

[0025]

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

[0026]

[0034] Referring to FIGS. 2 and 4 - 5, in this embodiment, the plurality of elongated walls 126a - 126d at the bottom edge or rim are present in or fit into corresponding grooves 113a - 113d on the upper surface of the bottom wall 112. Optionally, on the lower surface of the lid 116, there are a plurality of grooves 117a - 117d. In one or more embodiments, in the absence of the dispensing element 134, the plurality of elongated walls 126a - 126d at the upper end or rim can be present in or fit into the corresponding grooves 117a - 117d. The elongated walls 126a - 126d extend to the bottom wall 116 and, optionally, extend towards the lid 112 up to the height of the cavity that extends into the lid 112. The elongated walls are effective in conducting heat from one or more external sources.

[0027]

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

[0028]

[0036] The dispensing element can be of a suitable material or configuration or dimension or media grade that provides one or more of the following characteristics: namely, being able to withstand long - term exposure to the precursor, not inducing a pressure drop that would impede the effective delivery of the precursor, having a pore size that suppresses and / or prevents the microparticles and / or droplets of the precursor from exiting the ampoule to protect both the inlet and outlet devices, and being flexible enough to slightly seal the space between the end of the elongated wall and the inner diameter of the cavity. In one or more embodiments, the dispensing element is a porous disk of filter media. In one or more embodiments, the dispensing element is a sintered porous stainless steel material. The non - limiting and exemplary porosity of the dispensing element can be, as measured by the average pore size, from 0.1 μm or more to less than 100 μm, all values and sub - ranges therebetween.

[0029]

[0037] Further, there is an optional shim between the lower surface of the dispensing element and the upper edge of the elongated wall. The shim will be described in more detail with respect to shim 236 in FIG. 6.

[0030]

[0038] In some embodiments, the ampoule 100 includes a low vapor pressure material 150 within a cavity 118 that is present in a flow channel defined by elongated walls 126a-126d. The space above the material within the cavity 118 and below the lower surface of the lid is referred to as the headspace of the ampoule 100. When a dispensing element 134 is present, it is disposed within the headspace of the ampoule. The 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] In some embodiments, as shown in FIG. 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 container 110 using removable bolts through openings of appropriate shape and may have threads to facilitate connection of screw-type bolts. By removing the bolts, the lid 116 can be removed from the container 110 to change or add a precursor 150 within the container 110.

[0032]

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

[0033]

[0041] The first seal 152 is located between the upper surface of the side wall 114 and the lower surface of the lid 116 and forms a fluid-tight seal. The second seal 154 is located between the upper portion of the bottom wall 112 and the lower surface of the side wall 114 and forms 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 can be integrally formed with the side wall 114 and the bottom wall 112 of the container 110.

[0035]

[0043] To enable adding the ampoule 100 to the processing chamber, different manifold configurations can be connected to the lid 116. 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 positioned 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 external environment of the container 110. In some embodiments, there are a plurality of valves along the inlet line 170 (e.g., 174) and / or the outlet line 180 (e.g., 184) and / or therebetween (e.g., 190). The valves can be manual valves or pneumatic valves.

[0036]

[0044] FIG. 3 shows a top perspective view of the elongated walls 126a - 126d of an ampoule having flow annotations according to one or more embodiments. In one or more embodiments, the elongated walls 126a - 126d include an elongated tubular wall that defines a series of flow channels 124a - 124e. As depicted in FIG. 3, in one or more embodiments, the elongated walls 126a - 126d are concentric tubes. The relative positions of the walls can be adjusted, for example, to advantageously act on the reduction of precursors in a desired matter. In one or more embodiments, the annular distance between the walls varies. Using tubular elongated walls made by nesting readily available tubes facilitates assembly and can reduce the cost of the ampoule.

[0037]

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

[0038]

[0046] Therefore, the flow channels 124a to 124e are nested and include a plurality of meandering passages (124a, 124b, 124c, 124d) and an outlet passage (124e). With respect to the meandering passages, the flow passing through the first inlet openings (128a, 128b, 128c) deflects the carrier gas into first and second portions flowing in first and second directions (e.g., B1 and B2, C1 and C2, and D1 and D2) through the first and second sections of the meandering passages, respectively.

[0039]

[0047] FIG. 1B shows a schematic view of an ampoule and an accompanying manifold having an "inside-to-outside flow" configuration according to an embodiment. The ampoule 200 and the manifold 202 are suitable for use with semiconductor manufacturing materials including reagents and precursors. The term "precursor" is used to describe the contents of the ampoule 200 and means any reagent flowing into the processing environment.

[0040]

[0048] The ampoule 200 includes a container 210 having a bottom wall 212, side walls 214, and a lid 216. The inlet port 220 and the outlet port 230 are in fluid communication with a cavity defined by the inner wall of the container 210. The inlet port 220 is generally configured to allow connection to a gas source "G" by appropriate piping and valve(s) and can have an appropriate threaded or sealed connection. In one or more embodiments, the gas source "G" is a carrier gas, and in one or more embodiments, the carrier gas is inert. Also, the outlet port 230 is in fluid communication with the cavity. The outlet port 230 is generally configured to be connectable to a line including appropriate piping and valve(s) for flowing a gas stream that may contain particles entrained with droplets out of the container 210 to a processing chamber (or other component) "P". The outlet port 230 may have a welded connection or a threaded connection to allow connection of a gas line.

[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] Referring to the embodiment of FIG. 6 showing a partial perspective cross-section of the ampoule and the manifold of FIG. 1B, the ampoule includes a single inlet port 220 and a single outlet port 230. In the embodiment of FIG. 6, one inlet port and one outlet port are depicted respectively, but if specific applications require, there may be multiple inlet ports and outlet ports. By swapping the positions of the inlet and outlet, it is also possible to adapt to other designs.

[0043]

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

[0044]

[0052] The outlet port 230 has a passage 231 that extends into a part of the lid 216 in the depth direction and has an inner diameter that defines the cross-sectional width of the passage 231. The passage 231 is in fluid communication with the outlet port plenum 232. The outlet port plenum 232 is designed to accommodate the volume of the carrier gas that is entrained and / or saturated and flows out, and this carrier gas then flows out from the ampoule into the downstream processing chamber "P". The outlet port plenum 232 is sized such that it does not restrict the flow of the carrier gas that is entrained and / or saturated and flows out. The outlet port plenum 232 may be positioned and / or sized to accommodate the outflow flow line.

[0045]

[0053] Specifically describing the present embodiment, the cavity 218 is composed of a plurality of flow channels 224a to 224e defined by a plurality of elongated walls 226a to 226d. Each of the elongated walls 226a to 226d is provided with an inlet opening such as the inlet opening 228a of the wall 226a, the inlet opening 228b of the wall 226b, the inlet opening 228c of the wall 226c, and the inlet opening 228d of the wall 226d. The inlet openings are offset so that one inlet opening does not overlap with another inlet opening.

[0046]

[0054] In one or more embodiments, the plurality of elongated walls 226a to 226d at the bottom edge or rim may be present in or fit into corresponding grooves (not shown in FIG. 6 but similar to 113a to 113d) on the upper surface of the bottom wall 212. In this embodiment, there are no grooves on the lower surface of the lid 216. The elongated walls 226a to 226d extend to the bottom wall 216 and spread up to the height of the cavity towards the lid 212. The elongated walls are effective in conducting heat from one or more external sources.

[0047]

[0055] A distribution element 234, characterized as such with respect to the distribution element 134 of FIGS. 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, the flow exiting the inlet plenum 222 passes through the distribution element 234 before entering the cavity 218, and the flow exiting the cavity 218 passes through the distribution element 234 before entering the outlet plenum 232.

[0048]

[0056] In the embodiment of FIG. 6, a shim 236 is disposed 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 in order not to restrict the flow. The shim is a soft and conformable material such as a soft metal like aluminum, a flexible polymer material, or an elastomer material. The shim provides a supporting force to the distribution element 234.

[0049]

[0057] In some embodiments, the ampoule 200 contains a low vapor pressure material within the cavity 218 that is present in a flow channel defined by the elongated walls 226a-226d. The space above the material within the cavity 218 and below the lower surface of the lid is referred to as the headspace of the ampoule 200. When the dispensing element 234 is present, it is disposed within the headspace of 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 FIG. 6, the lid 216 is a separate component from the bottom wall (e.g., 212 of FIG. 1A) and the side wall 214. The lid 216 can be connected to the side wall 214 of the container using removable bolts through appropriately shaped openings and may have threads to facilitate connection of threaded bolts. The bolts can be removed to remove the lid 216 from the container so that the precursor within the container can be changed or added.

[0051]

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

[0052]

[0060] The first seal 252 is located between the upper surface of the side wall 214 and the lower surface of the lid 216 and forms a fluid tight seal. A second seal for forming a fluid tight seal is disposed between the upper portion of the bottom wall and the lower surface of the side wall. 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 can be integrally formed with the side wall 214 and the bottom wall of the container.

[0054]

[0062] As discussed with respect to FIG. 2, different manifold configurations can be connected to the lid 216 such that the ampoule 200 can be added to the processing chamber.

[0055]

[0063] FIG. 7 shows a top perspective view of the elongated walls 226a - 226d of an ampoule with flow annotations according to one or more embodiments. In one or more embodiments, the elongated walls 226a - 226d include elongated tubular walls that define a series of flow channels 224a - 224e. As depicted in FIG. 7, in one or more embodiments, the elongated walls 226a - 226d are concentric tubes. The relative positions of the walls can be adjusted, for example, to advantageously act on the reduction of precursors in a desired substance. In one or more embodiments, the annular distance between the walls varies. By using tubular elongated walls made by nesting readily available tubes, assembly is facilitated and the cost of the ampoule can be reduced.

[0056]

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

[0057]

[0065] Therefore, the flow channels 224a to 224e are nested and include a plurality of meandering passages (224e, 224d, 224c, 224b) and an outlet passage (224a). With respect to the meandering passages, the flow passing through the first inlet openings (228d, 228c, 228b) deflects the carrier gas in first and second directions (e.g., F1 and F2, G1 and G2, H1 and H2) that flow through the first and second sections of the meandering passages, respectively.

[0058]

[0066] According to one or more embodiments, the inlet openings of any embodiment are suitable for allowing the carrier gas to flow from one flow channel to another. The inlet openings can take any suitable shape and / or configuration and / or position along the elongated wall to accommodate the flow of droplet-laden and / or saturated carrier gas. The inlet openings may extend along the entire length of the container or may vary in length. The features of the inlet openings can be a plurality of holes, tapered slots, or other shapes. In one or more embodiments, the size and shape of the inlet openings are determined such that the conductance of the carrier gas varies along the longitudinal distance of the container. In one or more examples, the size of the inlet opening(s) increases 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 inlet opening 328 that extends along the length of the elongated wall, increases in size from the lid edge 330 to the bottom wall edge 332, and increases the conductance from the lid towards the bottom wall of the ampoule.

[0059]

[0067] In one or more embodiments, the inlet opening is a notch located at the upper end of the elongated wall near the lid. In one or more embodiments, each of the inlet openings extends for a longitudinal distance of from 1 to 5% or more to 100% or less of the length of the wall, including all values and partial ranges therebetween.

[0060]

[0068] In one or more embodiments, the inlet openings are a plurality of holes in each wall spaced along the length of each wall. In one or more embodiments, the plurality of holes spaced 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, this may depend on the specific precursor and its physical properties within the ampoule, but the carrier gas is expected to be fully saturated over the flow path distance. As the amount of precursor level in the ampoule decreases during use, the saturation may decrease. Saturation may vary as a function of the fill level.

[0062]

[0070] It is understood that the presence of the five flow channels in FIGS. 2-3 is not limiting, and the number of channels can be selected based on spatial constraints and / or precursor properties and / or design requirements.

[0063]

[0071] In some embodiments, the gas flow along the flow path through the inlet port 120 is sufficient to entrain the precursor and / or vaporize and / or sublime it without the need for bubbling. The gas flow can be adjusted during processing as the level of the precursor 150 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 equipment shown herein to monitor the processing conditions. In one or more embodiments, a mass flow meter is provided to monitor the gas flow to the inlet port. In one or more embodiments, a thermocouple is installed on the lid. In one or more embodiments, the pressure gauge is provided over the inlet line and / or the outlet line. The pressure range within the ampoule according to some embodiments is from 25 torr or more to 150 torr or less.

[0065]

[0073] Throughout this specification, references to "one embodiment", "certain embodiments", "one or more embodiments", or "an embodiment" mean that the particular features, structures, materials, or characteristics described in connection with the embodiment are included in at least one embodiment of the invention. Thus, the appearances of the phrases "in one or more embodiments", "in certain embodiments", or "in an embodiment" in various places throughout this specification are not necessarily referring 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] The present invention has been described with reference to particular embodiments, it should be understood that these embodiments are merely exemplary 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. Accordingly, the present invention is intended to cover modifications and variations that 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; An ampoule comprising:

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. 2. The ampoule of claim 1, wherein each of the entry openings progresses along a length of the elongated wall such that the opening size increases from a lid edge to a bottom wall edge.

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 walls including an entrance opening, the entrance openings being offset such that one entrance opening does not overlap another entrance 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; An ampoule comprising:

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 progresses along a length of the elongated wall such that the opening size increases from a lid edge to a bottom wall edge of the elongated wall.

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 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; The method includes:

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. 20. 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 that flow in first and second directions, respectively, through first and second sections of the passage.

Images