Ampoule for semiconductor manufacturing precursors

Abstract

Ampules for semiconductor fabrication precursors and methods of using the same are described. The ampoule includes a container having an air inlet port and an air outlet port. The ampoule includes an air inlet plenum between the air inlet port and the cavity and an air outlet plenum between the air outlet port and the cavity. A flow path is defined by a plurality of tubular walls and a flow intake opening of the ampoule adjacent a bottom edge of the tubular walls through which a carrier gas flows in contact with the precursor.

Description

Technical Field

[0001] The present invention generally relates to ampoules and methods for delivering semiconductor manufacturing precursors to a semiconductor processing chamber. In certain embodiments, the present invention relates to ampoules and methods that provide a tortuous flow path for low vapor pressure precursors. Background Art

[0002] The semiconductor industry is using an increasing number of liquid and solid precursors (also referred to as "chemicals") for chemical vapor deposition (CVD) and atomic layer deposition (ALD) processes. Precursors or chemicals are typically located within a closed container or ampoule having a single inlet and a single outlet, and the precursors are typically delivered in vapor form to a semiconductor processing chamber using a carrier gas.

[0003] Precursors having a low vapor pressure typically utilize a carrier gas to carry precursor vapor from the ampoule to a semiconductor processing chamber for a vapor deposition process. These types of processes typically use two types of ampoules: bubblers, where the inlet carrier gas enters a tube immersed in the precursor; and cross-flow ampoules, where the carrier gas sweeps across the headspace within the ampoule. Typically, the carrier gas has a very short flow path. The short flow path from the inlet to the outlet of the container does not allow sufficient residence time within the container for the carrier gas to be fully saturated with the vaporized or sublimed precursor. Some existing ampoule designs do not distribute the carrier gas evenly across the entire surface of the precursor. Some existing ampoule designs do not provide sufficient heating of the precursor throughout the container. Many other solid source ampoules do not provide a means to prevent the propagation of precursor dust downstream, thereby impeding the performance of control valves or creating particulate problems on the wafers.

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

[0005] One or more embodiments relate to an ampoule for a semiconductor manufacturing precursor. The ampoule includes a container defining a cavity configured to receive a precursor and bounded by a sidewall, a lid assembly, and a bottom wall. An inlet port and an outlet port are each in fluid communication with the cavity. The ampoule includes an inlet gas chamber located between the inlet port and the cavity and an outlet gas chamber located between the outlet port and the cavity. A plurality of elongate walls each have a defined length and are configured with a top edge and a bottom edge to receive the precursor, and the plurality of elongate walls are arranged to define a flow channel. Each elongate wall includes an inlet opening extending from the bottom edge. The flow path is defined by the flow channel and the flow inlet openings, through which the carrier gas flows in contact with the precursor.

[0006] Additional embodiments of the present invention relate to an ampoule for dispensing a vapor mixture of a carrier gas and a precursor, such as a low vapor pressure precursor used in semiconductor manufacturing. The ampoule includes a container having a bottom wall, a side wall, and a lid assembly that defines a cavity configured to receive the precursor such that the height (H) of the cavity spans from the lower surface of the lid assembly to the 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 gas chamber located between the inlet port and the cavity and an outlet gas chamber located between the outlet port and the cavity. A plurality of elongated tubular walls are configured to contain the precursor and are arranged to define a flow channel, each elongated wall having a defined length and a top edge and a bottom edge arranged to define the flow channel, each elongated wall including a flow inlet opening that extends from the bottom edge, the flow inlet openings being offset such that no one inlet opening overlaps another inlet opening. A tortuous flow path defined by the flow channel and the flow inlet openings through which the carrier gas flows to contact the precursor.

[0007] A further embodiment of the present invention relates to a method of providing a precursor flow in a substrate processing chamber during a chemical vapor deposition process to form a film on a substrate. The method includes flowing a carrier gas through an inlet port and an inlet gas chamber of an ampoule containing a low vapor pressure precursor. The carrier gas is directed within the ampoule and contacts the precursor through a flow path defined by a plurality of elongated walls having a top edge and a bottom edge and a flow inlet opening in each elongated wall, the carrier gas flowing through the flow inlet openings to contact the precursor, the flow inlet openings extending from the bottom edge of each of the plurality of elongated walls. The carrier gas and the precursor flow out of the ampoule through an outlet gas chamber and an outlet port into the substrate processing chamber. BRIEF DESCRIPTION OF THE DRAWINGS

[0008] To enable a detailed understanding of the above-described features of the present invention, a more specific description of the invention briefly summarized above may be had by reference to the embodiments, some of which are illustrated in the accompanying drawings. It should be noted, however, that the drawings illustrate only typical embodiments of the invention and should not be considered limiting of its scope, as the invention may admit to other equally effective embodiments.

[0009] Figure 1A is an isometric view of an ampoule and an attached manifold having an "outer-to-inner flow" configuration according to one embodiment;

[0010] Figure 1B is an isometric view of an ampoule and an attached manifold having an "inner-to-outer flow" configuration according to another embodiment;

[0011] Figure 2 is a perspective view of a lid of an ampoule according to one embodiment.

[0012] Figure 3A is according to one or more embodimentsFigure 1A taken along line 3-3 of Figure 1A sectional view;

[0013] Figure 3B is Figure 3A a partial sectional view of sectional area 3B in

[0014] Figure 3C is Figure 3A a partial sectional view of sectional area 3C in

[0015] Figure 3D is Figure 3A a partial sectional view of sectional area 3D in

[0016] Figure 4 is a bottom perspective view of the tubular wall of an ampoule according to one or more embodiments, showing an interpretation of the vapor flow; Figure 1A and Figure 3A

[0017] Figure 5 is an isometric view of the tubular wall according to an embodiment of the present disclosure;

[0018] Figure 6 is a perspective view of a filter insert including an orifice in an ampoule according to one or more embodiments, Figure 1A and Figure 3A

[0019] Figure 7A is a perspective view of a filter installed within a flange on the bottom side of an ampoule according to one or more embodiments, Figure 1A and Figure 3A

[0020] Figure 7B is Figure 7A a partial sectional view of sectional area 7B in

[0021] Figure 8 is a bottom perspective view of a cap assembly of an ampoule according to one embodiment;

[0022] Figure 9 is configured to be used with Figure 8 the cap assembly shown in a perspective view of an ampoule and a sheet;

[0023] Figure 10A is a sectional view of the cap assembly shown in Figure 11 assembled with a container according to an alternative embodiment;

[0024] Figure 10B is Figure 10A a partial sectional view of sectional area 10B in

[0025] Figure 10C yes Figure 10A a partial cross-sectional view of the middle cross-sectional area 10C;

[0026] Figure 10D yes Figure 10A a partial cross-sectional view of the mid-section area 10D;

[0027] Figure 10E yes Figure 10A a partial cross-sectional view of the mid-section region 10E; and

[0028] Figure 11 is a bottom perspective view of a cap assembly for an ampoule according to an alternative embodiment.

[0029] In the drawings, similar components and / or features may have the same reference number. Furthermore, various components of the same type may be distinguished by following the reference number with a dash and a second label that distinguishes the similar components. If only the first reference number is used in the specification, the description applies to any similar component having the same first reference number, regardless of the second reference number. Cross-hatching of components in the drawings is intended to aid visualization of the different components and does not necessarily indicate different materials of construction. DETAILED DESCRIPTION

[0030] Before describing several exemplary embodiments of the present disclosure, it should be understood that the present disclosure is not limited to the details of construction or process steps set forth in the following description. The claimed ampoules and methods are capable of other embodiments and of being practiced or carried out in various ways.

[0031] Some embodiments of the present invention advantageously provide a long flow path for the carrier gas from the ampoule inlet to the outlet for transporting low vapor pressure precursors, such as liquid and / or solid source precursors. Low vapor pressure precursors are understood to refer to materials that are not easily vaporized 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 is used to transport the low vapor pressure material from the ampoule to the 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 indium hafnium.

[0032] The long flow path within the ampoule containing the precursor allows the carrier gas sufficient residence time to partially become almost completely saturated with vaporized and / or sublimated and / or entrained precursor, which is a carrier of the carrier gas flowing through the ampoule. References herein to "saturated" allow for varying degrees of saturation.

[0033] 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. Some specific embodiments advantageously retain the low vapor pressure precursor comprising solid precursor dust within the cavity of the container, not allowing it to migrate upstream or downstream to the control valve. Some embodiments advantageously control the uneven consumption of the precursor. Some embodiments advantageously provide a uniform distribution of the carrier gas along the entire surface of the precursor. Embodiments herein provide improved dosages of precursors to substrate processing chambers, such as atomic layer deposition chambers and chemical vapor deposition chambers for depositing layers formed by the precursor onto substrates, such as semiconductor substrates and other substrates used in microelectronics manufacturing. The design provided herein can provide high capacity (volume) ampoules in a smaller footprint than other designs. The design herein is easy to clean and refill. The design herein can include up to 10-20 kilograms of precursor charge (i.e., the amount of precursor).

[0034] In some embodiments, the ampoule includes a plurality of elongated walls defining a labyrinth, such that the flow path is tortuous. Advantageously, one or more embodiments provide a flow path that can be five to ten times longer than that found in conventional ampoules, particularly solid source sublimation vessels. In one or more embodiments, the walls defining the labyrinth are formed of a solid material, such as a non-porous metal, and gas passing through the tortuous path flows only through flow inlet openings formed in the walls, and not through the wall itself.

[0035] Generally speaking, according to one or more embodiments, an ampoule includes a container defining a cavity configured to receive and hold a precursor; an inlet port and an outlet port, each in fluid communication with the cavity; an inlet plenum and an outlet plenum, each located between a corresponding inlet port or outlet port and the cavity; and a plurality of elongated walls containing the precursor, arranged to define flow channels, each elongated wall including a flow inlet opening. The walls are solid and non-porous, except for the flow inlet opening. A flow path is defined by the flow channels and the flow inlet openings, through which a carrier gas flows into contact with the precursor. In one or more embodiments, the flow path runs from the outermost channel to the innermost channel, which can be referred to as an "outside-to-inside flow" configuration. In one or more embodiments, the flow path runs from the innermost channel to the outermost channel, which can be referred to as an "inside-to-outside flow" configuration.

[0036] 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 flow channels, each flow channel containing a volume of solid precursor. The gas flow changes direction from one flow channel to another until it reaches the last flow channel that is connected to the outlet port. This change in direction also enhances the mixing of the vaporized and / or sublimated precursor with the carrier gas. The inlet opening allows the carrier gas to flow into the next flow channel. The gas flow referred to herein includes the carrier gas alone or in combination with the entrained and / or vaporized and / or sublimated precursor. For example, reference is made herein to Figure 3A 、 Figure 4 or Figure 10A Having described the flow path, it will be appreciated that a series of tubular or other elongated walls having inlets configured to define flow passages therebetween will produce the desired flow path. Preferably, the flow inlet openings are offset to ensure that no flow passages are bypassed.

[0037] Figure 1A A schematic diagram of an ampoule and accompanying manifold having an "outside-to-in flow" configuration is shown, according to one embodiment. Ampoule 100 and manifold 102 are suitable for use with semiconductor manufacturing feedstocks 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 processing environment.

[0038] The ampoule 100 includes a container 110 having a bottom wall 112, a side wall 114, and a lid assembly 116 including a lid 115. 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 typically configured to allow connection to a gas source "G" through suitable tubing and valves, and may have suitable threaded or sealed connections. In one or more embodiments, the gas source "G" is a carrier gas; in one or more embodiments, the carrier gas is inert. The outlet port 130 is also in fluid communication with the cavity. The outlet port 130 is typically configured to be connected to a line (including suitable tubing and valves) to allow a flow of gas, which may include entrained particles, to exit the container 110 to flow to a processing chamber (or other component) "P". The outlet port 130 may have a welded or threaded connection to allow connection of a gas line. The height (H) of the cavity defined by the container 110 spans from a lower surface 116 a of the lid assembly 116 to a top surface 112 a of the bottom wall 112 .

[0039] Steering Figure 2 , showing a schematic diagram of the bottom wall of the ampoule of the embodiment, and Figure 3A Shown Figure 1A In the cross-sectional view of FIG, the ampoule includes a single air inlet port 120 and a single air outlet port 130. Although Figure 3AThe embodiments depict each of the inlet port and the outlet port, but there may be multiple inlet ports and outlet ports if required by a particular application. The positions of the inlet and outlet can be swapped to accommodate other designs.

[0040] The inlet port 120 has a channel 121, the inner diameter of the channel 121 defining the cross-sectional width of the channel 121, and the channel 121 extends to a portion of the depth of the lid assembly 116. The channel 121 is in fluid communication with the inlet port plenum 122. The inlet port plenum 122 is designed to hold a quantity of incoming carrier gas from source "G", which in turn flows into the chamber - typically the chamber is shown as 118. The inlet port plenum 122 is sized so as not to restrict the flow of the incoming carrier gas. The position and / or size of the inlet port plenum 122 can accommodate the incoming flow line.

[0041] The outlet port 130 has a channel 131, the inner diameter of the channel 131 defining the cross-sectional width of the channel 131, and the channel 131 extends to a portion of the depth of the lid assembly 116. The channel 131 is in fluid communication with the outlet port plenum 132. The outlet port plenum 132 is designed to hold a volume of output entrained and / or saturated carrier gas, which in turn flows from the ampoule to the downstream processing chamber "P". The outlet port plenum 132 is sized so as not to restrict the flow of the outgoing entrained and / or saturated carrier gas. The position and / or size of the outlet port plenum 132 can accommodate the outgoing flow line.

[0042] Specifically, for the present embodiment, the chamber 118 consists of a plurality of flow channels 124a - 124e, the plurality of flow channels 124a - 124e being defined by a plurality of elongate walls 126a - 126d. Each of the elongate walls 126a - 126d includes a flow inlet opening as follows: the inlet opening 128a of the elongate wall 126a, the inlet opening 128b of the elongate wall 126b, the inlet opening 128c of the elongate wall 126c, and the inlet opening 128d of the elongate wall 126d. The flow inlet openings are offset such that one inlet opening does not overlap another inlet opening.

[0043] Reference Figure 2 and Figure 3AIn this embodiment, a plurality of elongated walls 126a-126d at the bottom edge or rim reside in or mate with corresponding recesses 117a-117d in the lower surface 116a of the lid assembly 116. A plurality of recesses 113a-d aligned with the recesses 117a-117d may optionally be present in the lower surface of the bottom wall 112. In one or more embodiments, in the absence of the dispensing element 134, the plurality of elongated walls 126a-126d at the top edge or rim may reside in or mate with a plurality of recesses (optionally) present in the lower surface of the lid assembly 116. The elongated walls 126a-126d span the height of the cavity, extending into the bottom wall 112 and toward and (optionally) into the lid 115. The elongated walls 126a-126d effectively conduct heat from one or more external heat sources. In an embodiment, the elongated walls are solid and non-porous, allowing gas to flow through the elongated walls 126a-126d at the gas inlet.

[0044] Optionally, there is a distribution element 134 sandwiched between the lid assembly 116 and the top edge of the elongated wall. The distribution element 134 is located between the cavity 118 and the inlet port plenum 122 and the outlet port plenum 132, respectively. That is, the flow exiting the inlet port plenum 122 passes through the distribution element 134 before entering the cavity 118, and the flow exiting the cavity 118 passes through the distribution element 134 before entering the outlet port plenum 132. Thus, the distribution element extends across the width or diameter of the container and covers the top surfaces of the walls 126a-d.

[0045] The distribution element 134 can be any suitable material or construction or size or media grade that provides one or more of the following properties: the ability to withstand extended exposure to the precursor, the induction of a pressure drop that would impede efficient delivery of the precursor, a pore size that inhibits and / or prevents fine particles and / or droplets of the precursor from exiting the ampoule, thereby protecting the inlet and outlet devices, and being flexible enough to form 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 134 is a porous disc of filter media. In one or more embodiments, the distribution element is a sintered porous stainless steel material. Non-limiting exemplary porosities of the distribution element 134 can be greater than or equal to 0.1 microns to less than 100 microns, and all values and subranges therebetween, as measured through the mean pore size. In some embodiments, there can be a gasket between the lower surface of the distribution element 134 and the top edge of the elongated wall.

[0046] In some embodiments, the ampoule 100 includes a precursor 150 which, in some embodiments, is a low vapor pressure material within the cavity 118 and present in the flow channels defined by the elongate walls 126a - 126d. The space above the material within the cavity 118 and below the lower surface 116a of the lid assembly is referred to as the headspace of the ampoule 100. When present, the dispensing element 134 is located within the headspace of the ampoule. The precursor 150 can be a precursor for semiconductor manufacturing processes. In one or more embodiments, the material having a low vapor pressure is a liquid. In other embodiments, the material having a low vapor pressure is a solid.

[0047] In some embodiments, as Figure 3A shown, the lid assembly 116 is a component separate from the bottom wall 112 and the side wall 114. The lid assembly 116 can be attached to the side wall 114 of the container 110 using removable bolts passing through appropriately shaped openings which can have threaded portions to allow for easy connection of threaded bolts. The removable bolts allow for the removal of the lid assembly 116 from the container 110 in order to replace or add the precursor 150 within the container 110.

[0048] The lid may also include one or more outer surface features for reciprocating movement with an external heater. The bottom wall can be configured for reciprocating movement with an external heater. One or more jacket heaters can be provided around the side wall.

[0049] A first seal 152 is located between the upper surface of the side wall 114 and the lower surface 116a of the lid assembly 116 to form a fluid - tight seal. In embodiments where the bottom wall 112 is a separately formed element, a second seal is located between the upper portion of the bottom wall 112 and the lower surface of the side wall 114 to form a fluid - tight seal. In Figure 3A the embodiment shown, the bottom wall 112 is integrally formed with the side wall 114, eliminating the need for a second seal. In some embodiments where the bottom wall 112 is a separately formed element, the first seal 152 and the second seal are independently O - rings. In some embodiments (not shown), the lid assembly 116 can be integrally formed with the side wall 114 and the bottom wall 112 of the container 110.

[0050] Different manifold configurations can be connected to the lid assembly 116 to allow the addition of the ampoule 100 to the processing chamber. In some embodiments, the inlet line 170 is connected to the inlet port 120. The inlet valve 172 can be positioned on the inlet line 170 between the gas source "G" and the inlet port 120. The inlet valve 172 can be formed integrally with the lid assembly 116 or connected to the lid assembly 116 as a separate component. The outlet line 180 can be connected to the outlet port 130. The outlet line 180 of 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 external to 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 between them (e.g., 190). The valves can be manual valves or pneumatic valves.

[0051] Figure 4 A bottom perspective view of the slender walls 126a - 126d of an ampoule with flow annotations is shown in accordance with one or more embodiments. In one or more embodiments, the slender walls 126a - 126d include slender tubular walls that define a series of flow channels 124a - 124e. As Figure 3A shown, in one or more embodiments, the slender walls 126a - 126d are concentric and tubular. The relative positions of the walls can be adjusted to (e.g.) facilitate the consumption of a precursor in a desired amount. In one or more embodiments, the annular distance between the walls varies. By nesting readily available tubes, it is beneficial for assembly and reduces the cost of the ampoule.

[0052] The carrier gas flows from the inlet port 120 through the inlet port gas chamber 122 into the ampoule 100, as regarding Figure 3AAs discussed. As shown by the dashed arrow "A" in Figure 3, the carrier gas enters the flow channel 124a defined by the side wall 114 and the elongated wall 126a, and after passing through the orifice 162, contacts the precursor 150 at a high speed, thereby entraining and / or vaporizing the precursor as the carrier gas passes over the surface of the precursor volume. The flow then continues 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 (as shown 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 travels 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 (as shown by arrows C1 and C2) through the flow channel 124c. While in 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 flow channel 124d and the surface of the elongated wall 126d directs the flow in two directions (as indicated by arrows D1 and D2) through flow channel 124d. While in flow channel 124d, the carrier gas continues to contact the precursor 150 and becomes saturated. Finally, the flow then continues through the inlet opening 128d of the elongated wall 126d, at which point the carrier gas enters flow channel 124e, as shown. Figure 3A As shown by the dotted arrow F in Figure 4 The carrier gas is shown by arrows E1 and E2 in FIG, and exits the ampoule through the outlet port 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.

[0053] Thus, the flow channels 124a-124e are nested, including a plurality of curved channels (124a, 124b, 124c, 124d) and an outlet channel or channels (124e) such that, relative to the curved channels, flow through the first inlet opening (128a, 128b, 128c) transfers the carrier gas into first and second portions, each portion flowing through the first and second portions of the curved channels, respectively, along first and second directions (e.g., B1 and B2, C1 and C2, and D1 and D2).

[0054] Figure 1B A schematic diagram of an ampoule and accompanying manifold having an "inside-out flow" configuration, according to an embodiment, is shown. Ampoule 200 and manifold 202 are suitable for use with semiconductor manufacturing feedstocks including reagents and precursors. The term "precursor" is used to describe the contents of ampoule 200 and refers to any reagent that flows into the processing environment.

[0055] The ampoule 200 includes a container 210 having a bottom wall 212, side walls 214, and a cap assembly 216. An inlet port 220 and an 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" through a suitable conduit and valve, and may have a suitable threaded or sealed connection. In one or more embodiments, the gas source "G" is a carrier gas; in one or more embodiments, the carrier gas is inert. The outlet port 230 is also in fluid communication with the cavity. The outlet port 230 is generally configured to be connectable to a pipeline, including suitable conduits and valves, to allow gas (which may include entrained particles) to leave the container 210 and flow to a processing chamber (or other component) "P". The outlet port 230 may have a welded or threaded connection to allow connection of a gas pipeline. The height (H) of the cavity defined by the container 210 extends from the lower surface 116a of the cap assembly 216 across to the top surface of the bottom wall 212.

[0056] It should be understood that, compared with the embodiments shown and discussed above with respect to Figure 3A and Figure 4 the flow of the gas and precursor entrained in the carrier gas through the embodiment shown in Figure 1B is substantially opposite. Thus, the flow is from the center of the ampoule, and the flow direction is opposite at arrows E1 and E2 in Figure 4 where the gas flows to the flow channel 124d and exits to the flow channel 124c at arrows D1 and D2 in the opposite direction as shown in Figure 4 and then exits to the flow channel 124b at arrows C1 and C2, where the flow is in the opposite direction as shown in Figure 4 and then through the opening 128a in the opposite direction of the arrows B1 and B2 as shown in Figure 4 . Then the precursor entrained in the gas flows to the outlet port 230 and flows to the processing chamber P, as shown in Figure 1B .

[0057] According to one or more embodiments, the flow inlet opening of any embodiment is adapted to allow the carrier gas to flow from one flow channel to another. The flow inlet opening may take any suitable shape and / or configuration and / or position along the elongate wall to accommodate the flow of the entrained and / or saturated carrier gas. The flow inlet opening may span the entire length of the container, or a different length. The flow inlet opening may be characterized by a plurality of holes, tapered slots, or other shapes. In one or more embodiments, the size and shape of the flow inlet opening are designed to provide a varying conductivity of the carrier gas along the longitudinal distance of the container. In one or more embodiments, the size of the flow inlet opening is increased to increase the conductivity from the cap assembly towards the bottom wall of the ampoule.

[0058] Now referring to Figure 5, an isometric view of a tubular wall 126a representative of each of the tubular walls 126a-d according to an embodiment of the present invention is shown. Each of the tubular walls 126a-d has a defined length L and is configured to receive a top edge 127 and a bottom edge 129 of a precursor, and a plurality of elongated walls are arranged to define a flow channel. Each elongated wall includes a flow inlet opening 128a having a dimension d that defines the longitudinal distance of the flow inlet opening 128a from the bottom edge 129 to the top of the inlet opening 128a.

[0059] In one or more embodiments, the flow inlet opening is a notch located at the bottom end of the elongated wall near the lid assembly. In one or more embodiments, the longitudinal distance d spanned by each flow inlet opening is greater than or equal to 1-5%, 1-10%, 1-20%, 1-30%, 1-40%, 1-50%, 5-10%, 5-20%, 10-20%, 5-30%, 10-30%, 15-30%, 5-40%, 10-40%, 20-40%, 5-50%, 10-50% or 25-50% to less than or equal to 100% of the length L of the tubular wall 126a, including all values and subranges therebetween.

[0060] In one or more embodiments, the flow inlet opening is a plurality of holes spaced along the length of each wall. In one or more embodiments, the size of the plurality of holes spaced along the length of each wall increases from the lid end edge to the bottom wall edge. In some embodiments, the flow inlet opening is in the form of a rectangular or substantially rectangular channel located at the bottom of each tubular wall. Substantially rectangular means that the transition from the horizontal edge to the vertical edge of the flow inlet opening does not necessarily have to be a right angle or a straight line, but can be curved. Simulation of the flow inlet opening at the bottom edge 129 of the tubular wall shows that for some precursors, the average efficiency is increased by +50%, up to 70%, compared to when the flow inlet opening is located near the top edge 127.

[0061] Now refer to Figure 6 , Figure 7A , Figure 7B , Figure 8 , and Figure 9As shown, embodiments of the present invention include a gas distribution insert 160 inserted into a container 135 or an opening of a dispensing element 134. The gas distribution insert 160 includes an orifice 162 therethrough, and the size and configuration of the orifice 162 are designed to increase the flow rate of gas flowing into the ampoule. In one or more embodiments, there is a single orifice 162, but any number of orifices may be present, such as 1 to 20 orifices or 1 to 6 orifices, each orifice having a diameter in the range of 0.01 mm to 10 mm, 0.01 to 1 mm, 0.2 mm to 0.9 mm, 0.2 to 0.8 mm, 0.3 mm to 0.7 mm to increase the carrier gas flow rate into the ampoule. The gas distribution insert 160 may also include fastener openings 160a and 160b to allow the insert 160 to be fastened to the dispensing element 134 or otherwise fastened to the cap assembly 116, as Figure 3B and Figure 8 shown, where the gas distribution insert 160 is fastened to the cap 115 at the container 135a.

[0062] The cap 115 includes a peripheral edge 111 having a plurality of threaded openings 101 to receive fasteners (such as bolts or other suitable fasteners) to secure the cap 115 to the container 110. Additionally, the peripheral edge 111 includes a pin socket 103 configured to receive a complementary pin 119 extending from the peripheral edge 111. The peripheral edge 111 includes an inward protrusion 105 that aligns and engages with a notch 107 in the dispensing element 134. The peripheral edge 111 also includes an external notch 109 that may further assist in aligning the dispensing element 134 and the peripheral edge 111. Figure 7B A complementary socket 135a aligned with a socket 135 in the dispensing element 134 is shown. Figure 8 A gas distribution insert assembled to the cap 115 is shown.

[0063] Now referring to Figure 10A -E and Figure 11 , an alternative embodiment of an ampoule 300 and a cap assembly 316 is shown. The ampoule 300 and the cap assembly 316 are suitable for use with semiconductor manufacturing materials including reagents and precursors. Details are not repeated for Figure 1A , Figure 2 , Figure 3A and Figure 4 since the overall construction of the ampoule 300 and the cap assembly 316 is generally similar to the ampoule 100 and the cap assembly 116 shown and described with respect to Figure 1A , Figure 2 , Figure 3A and Figure 4 . Details of the cap assembly 316 are as shown in Figure 11 which is the same as Figure 3Ais different from the lid assembly in that it includes a distribution element 334 assembled within the outlet gas chamber 332, rather than extending across the width or diameter of the container and covering the top surfaces of the walls 126a-d. Thus, the distribution element 134 is only located within the outlet gas chamber 332. The flow leaving the chamber 318 passes through the distribution element 334 before entering the outlet gas chamber 332. The distribution element 334 is held in place by a retaining element 337, which can be fastened to the lid by a fastener such as a screw or bolt. The gas distribution insert 360 includes an aperture 362 therethrough, and the aperture 362 is sized and configured to increase the flow rate of the gas flowing into the ampoule. In one or more embodiments, there is a single aperture 362, but any number of apertures can be present, such as 1 to 20 apertures or 1 to 6 apertures, each aperture having a diameter in the range of 0.01 mm to 10 mm, 0.01 to 1 mm, 0.2 mm to 0.9 mm, 0.2 to 0.8 mm, 0.3 mm to 0.7 mm to increase the carrier gas flow rate into the ampoule.

[0064] The distribution element 334 can be of any suitable material or construction or size or media grade that provides one or more of the following characteristics: withstand long-term exposure to the precursor, do not introduce a pressure drop that would impede the effective delivery of the precursor, the pore size of the precursor to inhibit and / or prevent fine particles and / or droplets of the precursor from leaving the ampoule to protect the inlet and outlet devices, and be flexible enough to form a slight seal between the end of the elongated wall and the inner diameter of the chamber. In one or more embodiments, the distribution element 334 is a porous disk of filter media. In one or more embodiments, the distribution element 334 is a sintered porous stainless steel material. A non-limiting exemplary porosity of the distribution element 334 can be greater than or equal to 0.1 micron to less than 100 microns, and all values and sub-ranges therebetween, as measured by the average pore diameter. Figure 11 The illustrated embodiment of the lid 315 also includes complementary pins 319 extending from the peripheral edge of the lid 315. Figure 11 The illustrated embodiment of the lid assembly 316 also includes a container 335a for receiving the gas distribution insert 360. A gasket 333 is disposed between the lower surface of the lid 315 and the top edges of the elongated walls 326a, 326b, 326c, and 326d. The gasket 333 is a sheet of soft and compliant material, such as a soft metal like aluminum, or a flexible polymer or elastomeric material such as polytetrafluoroethylene.

[0065] The ampoule 300 includes a container 310 having a bottom wall 312, a side wall 314, and a cap assembly 316 including a cap 315. An inlet port 320 and an outlet port 330 are in fluid communication with a cavity 313 defined by the inner wall of the container 310. The inlet port 320 is generally configured to allow connection to a gas source through a suitable conduit and valve and may have a suitable threaded or sealed connection. In one or more embodiments, the gas source is a carrier gas; in one or more embodiments, the carrier gas is inert. The outlet port 330 is also in fluid communication with the cavity 318. The outlet port 330 is generally configured to be connectable to a pipeline, including suitable conduits and valves, to allow a gas stream, which may include entrained particles, to leave the container 310 and flow to a processing chamber (or other component). The outlet port 330 may have a welded or threaded connection to allow connection of the gas pipeline. The height (H) of the cavity defined by the container 310 extends from the lower surface 316a of the cap assembly 316 across to the top surface of the bottom wall 312, as shown in the previous embodiments.

[0066] The cavity 318 is composed of a plurality of flow channels 324a, 324b, 324c, 324d, and 324e defined by a plurality of elongated walls 326a - 126d. Each of the elongated walls 326a, 326b, 326c, and 326d includes a flow inlet opening as follows: an inlet opening 328a of wall 326a, an inlet opening 328b of wall 326b, an inlet opening 328c of wall 326c, and an inlet opening 328d of wall 326d. The flow inlet openings are offset such that one inlet opening does not overlap with another inlet opening.

[0067] The plurality of elongated walls 326a - 326d at the bottom edge or edge are located in or mate with corresponding grooves in the lower surface of the cap assembly 316 (similar to the embodiment shown with respect to Figure 3A the embodiment shown). A plurality of grooves 313a - 313d (in Figure 10AOnly the grooves 313b and 313c can be seen because the grooves 313a and 313d are covered by the precursor) Optionally present in the lower surface of the bottom wall 312. In the illustrated embodiment, the top edges of the elongate walls 326a - 326 abut the gasket 333, and the gasket 333 is sandwiched between the top edges of the elongate walls 326a - 326d and the lid 315. In one or more embodiments, in the absence of the gasket 333, the top edges or multiple elongate walls 326a - 326d at the edges can reside in or cooperate with multiple grooves optionally present in the lower surface of the lid assembly 316. The elongate walls 326a - 326d span the height of the cavity, extend into the bottom wall 312 and towards the lid 315 and optionally into the lid 315. The elongate walls 326a - 326d effectively conduct heat from one or more external sources. In an embodiment, the elongate walls are solid and non - porous, allowing gas to flow over the elongate walls 326a - 326d at the intake openings.

[0068] As described above, there is a dispensing element 334. The dispensing element 334 is located between the cavity 318 and the outlet gas chamber 332. That is, the flow leaving the outlet gas chamber 332 passes through the dispensing element 334 before leaving the cavity 318 through the outlet gas chamber 332.

[0069] In some embodiments, the ampoule 300 includes a precursor 350, which in some embodiments is a low - vapor - pressure material within the cavity 318, residing in the flow channels defined by the elongate walls 326a - 326d. The space above the material within the cavity 318 and below the lower surface 316a of the lid assembly is referred to as the headspace of the ampoule 300. When present, the dispensing element 334 is located in the headspace of the ampoule. The precursor 350 can be a precursor for semiconductor manufacturing processes. In one or more embodiments, the material with low vapor pressure is a liquid. In other embodiments, the material with low vapor pressure is a solid.

[0070] In some embodiments, the lid assembly 316 is a component separate from the bottom wall 312 and the side wall 314. The lid assembly 316 can be connected to the side wall 314 of the container 310 using removable bolts through appropriately shaped openings, which can have threaded portions to allow for easy connection of threaded bolts. The removable bolts allow the lid assembly 316 to be removed from the container 310, so that the precursor 150 in the container 110 can be replaced or added.

[0071] The lid 315 can also include one or more outer surface features for reciprocating movement with an external heater. The bottom wall can be configured to reciprocate with an external heater. One or more jacket heaters can be provided around the side wall.

[0072] The first seal 352 is located between the upper surface of the side wall 314 and the lower surface 316a of the lid assembly 316 to form a fluid-tight seal. In embodiments where the bottom wall 312 is a separately formed element, a second seal is located between the upper portion of the bottom wall 312 and the lower surface of the side wall 314 to form a fluid-tight seal. In Figure 10A the illustrated embodiment, the bottom wall 312 is integrally formed with the side wall 314, eliminating the need for a second seal. In some embodiments where the bottom wall 312 is a separately formed element, the first seal 352 and the second seal are independently O-rings. In some embodiments (not shown), the lid assembly 316 may be integrally formed with the side wall 314 and the bottom wall 312 of the container 310.

[0073] Different manifold configurations may be connected to the lid assembly 316 to allow the addition of the ampoule 300 to the processing chamber. In some embodiments, an inlet gas line is connected to the inlet port 320 (similar to Figure 1A that shown). An inlet valve may be positioned in the inlet gas line between the gas source and the inlet port 320. The inlet valve may be integrally formed with the lid assembly 316 or connected to the lid assembly 316 as a separate component. An outlet gas line may be connected to the outlet port 330 (similar to Figure 1A that shown). The outlet gas line of some embodiments includes an outlet valve located between the outlet port 330 and the processing chamber. The inlet valve and the outlet valve may be used to isolate the ampoule 300 such that the contents of the chamber 318 are isolated from the environment external to the container 310. In some embodiments, multiple valves are present along the inlet gas line and / or the outlet gas line and / or between them (similar to Figure 1A that shown). The valves may be manual valves or pneumatic valves.

[0074] In one or more embodiments, the elongate walls 326a, 326b, 326c, and 326d include elongate tubular walls that define a series of flow channels 324a, 324b, 324c, 324d, and 324e. In one or more embodiments, the elongate walls 326a, 326b, 326c, and 326d are concentric and tubular. The relative positions of the walls may be adjusted to, for example, facilitate the consumption of precursors in the desired substance. In one or more embodiments, the annular distance between the walls varies. The use of tubular elongate walls fabricated by nesting readily available tubing facilitates assembly and reduces the cost of the ampoule.

[0075] The carrier gas flows from the inlet 320 through the inlet gas chamber 322 into the ampoule 300. As Figure 10AThe carrier gas indicated by the dashed arrow “A” enters the flow channel 324a defined by the side wall 314 and the elongated wall 326a and contacts the precursor 350 at high speed after passing through the orifice 362, thereby entraining and / or vaporizing the precursor as the carrier gas passes over the surface of the volume of the precursor. The flow then continues through the intake opening 328a of the elongated wall 326a, at which point the carrier gas enters the flow channel 324b, and the surface of the elongated wall 326b opposite the flow intake opening 328a guides the flow through the flow channel 324b in two directions, as indicated by arrows B1 and B2 (similar to the embodiment shown in Figure 4 ; ( Figure 10A arrow B2 shown in Figure 4 ). When in the flow channel 324b, the carrier gas continues to contact the precursor 350 and becomes saturated. Similarly, the flow then travels through the intake opening 328b of the elongated wall 326b, at which point the carrier gas enters the flow channel 324c and the surface of the elongated wall 326c guides the flow through the flow channel 324c in two directions, as indicated by arrows C1 and C2 (similar to the embodiment shown in Figure 10A ; ( Figure 4 arrow C2 shown in Figure 10A ). When in the flow channel 324c, the carrier gas continues to contact the precursor 350 and becomes saturated. Likewise, the flow then travels through the intake opening 328c of the elongated wall 326c, at which point the carrier gas enters the flow channel 324d and the surface of the elongated wall 326d guides the flow through the flow channel 324d in two directions, as indicated by arrows D1 and D2 (similar to the embodiment shown in Figure 10A ; ( Figure 4 arrows E1 and E2 depicted in the embodiment of Figure 10A in which arrow E2 is shown)), and exits the ampoule through the outlet gas chamber 332 and the outlet port 330. When in the flow channel 324e, the carrier gas continues to contact the precursor 350 and becomes saturated.

[0076] Thus, the flow channels 324a - 324e are nested to include a plurality of curved channels (324a, 324b, 324c, 324d) and an outlet flow channel or channels (324e) such that, relative to the curved channels, the flow through the first inlets (328a, 328b, 328c) transfers the carrier gas into first and second portions, each portion flowing in first and second directions (e.g., B1 and B2, C1 and C2, and D1 and D2) through first and second portions of the curved channels, respectively.

[0077] According to one or more embodiments, it is expected that the carrier gas will become fully saturated over the flow path distance when the ampoule contains a minimum amount of precursor, which may depend on the specific precursor in the ampoule and its physical properties. As the amount of precursor in the ampoule decreases during use, the saturation may decrease. The saturation may vary with the change in the fill level. It should be understood that the presence of the five flow channels as shown in the embodiments described herein is not restrictive, and the number of channels can be selected based on space limitations and / or precursor characteristics and / or design requirements.

[0078] In some embodiments, gas flows through the inlet port 120 or 320 and along the flow path for a sufficient distance to entrain and / or vaporize and / or sublime the precursor without the need for bubbling. When the level of the precursor 150 or 350 decreases, the gas flow can be adjusted during processing to maintain sufficient contact. In one or more embodiments, the flow has a maximum velocity sufficient to prevent condensation of the precursor 150 or 350 at the outlet port 130 or 330 when combined with a heat source.

[0079] A thermocouple, a mass flow meter, and a pressure gauge may be included in the apparatus represented herein to monitor the processing conditions. In one or more embodiments, a mass flow meter is provided to monitor the gas flow into the inlet port. In one or more embodiments, the thermocouple is mounted in the lid assembly. In one or more embodiments, the pressure gauge is provided on the inlet line and / or the outlet line. The pressure range within the ampoule according to some embodiments is greater than or equal to 25 Torr and less than or equal to 150 Torr.

[0080] 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 the embodiment is included in at least one embodiment of the present invention. Thus, appearances of the phrases such as "in one or more embodiments", "in certain embodiments", "in one embodiment" or "in an embodiment" throughout the specification are not necessarily referring to the same embodiment of the present invention. Furthermore, in one or more embodiments, the particular features, structures, materials, or characteristics may be combined in any manner.

[0081] Although the present invention has been described herein with reference to specific 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 of ordinary skill 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 present 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. An ampoule for a semiconductor manufacturing precursor, the ampoule comprising: A container that defines a cavity configured to hold the precursor; An inlet port and an outlet port, both the inlet port and the outlet port being in fluid communication with the cavity; An inlet gas chamber located between the inlet port and the cavity; An outlet gas chamber located between the outlet port and the cavity; A plurality of elongated walls having a top edge and a bottom edge that define a length and are configured to hold the precursor, the plurality of elongated walls being arranged to define a flow channel, each elongated wall including a flow inlet opening; And A flow path defined by the flow channel and the flow inlet opening, through which a carrier gas flows into contact with the precursor.

2. The ampoule of claim 1, wherein the plurality of elongated walls and the inlet openings define a labyrinth seal such that the flow path is curved.

3. The ampoule of claim 1, wherein the flow inlet openings are offset such that no inlet opening overlaps another inlet opening.

4. The ampoule of claim 1, wherein the ampoule includes a single inlet port and a single outlet port.

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

6. The ampoule of claim 1, further comprising a distribution element located between the cavity and only the outlet gas chamber.

7. The ampoule of claim 1, wherein the plurality of elongated walls comprise a solid non-porous material.

8. The ampoule of claim 1, wherein there is an orifice between the inlet port and the cavity, the orifice being configured to increase the flow rate of the gas flowing through the orifice.

9. An ampoule for dispensing a vapor mixture of a carrier gas and a low vapor pressure precursor used in semiconductor manufacturing, the ampoule comprising: A container having a bottom wall, a plurality of side walls, and a lid assembly, the container defining a cavity configured to hold the precursor such that the height (H) of the cavity spans from the lower surface of the lid assembly to the top surface of the bottom wall; A single inlet port and a single outlet port, both the single inlet port and the single outlet port being in fluid communication with the cavity; An inlet gas chamber located between the inlet port and the cavity; An outlet gas chamber located between the outlet port and the cavity; A plurality of elongated tubular walls configured to hold the precursor and arranged to define a plurality of flow channels, each elongated tubular wall having a top edge and a bottom edge that define a length and being arranged to define a flow channel, each elongated tubular wall including a flow inlet opening that extends from the bottom edge, the flow inlet openings being offset such that no inlet opening overlaps another inlet opening; And A curved flow path defined by the flow channels and the flow inlet openings, through which a carrier gas flows into contact with the precursor.

10. The ampoule according to claim 9, wherein the ampoule further comprises a dispensing element located between the cavity and both the inlet gas chamber and the outlet gas chamber, and spanning at least a distance of the inner diameter defined by the side wall.

11. The ampoule according to claim 9, wherein the ampoule further comprises a dispensing element located between the cavity and only the outlet gas chamber.

12. The ampoule according to claim 9, wherein the plurality of elongated tubular walls are concentric and made of solid non-porous material.

13. The ampoule according to claim 9, wherein the bottom wall comprises a plurality of grooves that cooperate with the plurality of elongated tubular walls.

14. The ampoule according to claim 9, wherein there is an orifice between the inlet port and the cavity, and the orifice is configured to increase the flow rate of the gas flowing through the orifice.

15. The ampoule according to claim 14, wherein the diameter of the orifice is in the range of 0.3 mm to 0.7 mm.

16. The ampoule according to claim 9, wherein the flow channels are nested, and the flow channels comprise: A plurality of curved channels and an outlet channel, such that relative to the curved channels, the flow through the first inlet opening transfers the carrier gas to a first portion and a second portion and flows through the first portion and the second portion of the curved channels along a first direction and a second direction, respectively.

17. A method of providing a precursor flow in a substrate processing chamber during a chemical vapor deposition process to form a film on a substrate, the method comprising: Flowing a carrier gas through an inlet port and an inlet gas chamber of an ampoule containing a precursor having a low vapor pressure; Directing the flow of the carrier gas to flow within the ampoule and contact the precursor through a flow path defined by a plurality of elongated walls having a top edge and a bottom edge and a flow inlet opening in each of the elongated walls, the carrier gas flowing through the flow path to contact the precursor, and the flow inlet opening extending from the bottom edge of each of the plurality of elongated walls; and Flowing the carrier gas and the precursor out of the ampoule, through an outlet gas chamber and an outlet port, into the substrate processing chamber.

18. The method according to claim 17, the method further comprising: Directing the gas flow through an orifice configured to increase the flow rate of the carrier gas contacting the precursor.

19. The method according to claim 17, the method further comprising: Independently heating a lid assembly and a bottom wall of the ampoule, and the plurality of elongated walls effectively conduct heat from an external heat source.

20. The method according to claim 17, wherein the flow path comprises nested channels such that the flow through the first inlet opening diverts the carrier gas to a first portion and a second portion and flows through the first portion and the second portion of the channels along a first direction and a second direction, respectively.

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