Multi-chamber chemical solid precursor ampoule

Abstract

A multi-chamber ampoule is disclosed, which includes a multi-chamber container and a lid. The lid includes a conduit for fluidly connecting the multiple chambers of the container. The sublimation rate of each chamber is determined by the surface area of ​​each chamber, the temperature of each chamber, and the headspace pressure of each chamber, and the sublimation rate of each chamber is substantially equal.

Description

[Technical Field]

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS This application claims the benefit of U.S. Provisional Patent Application No. 63 / 489,290, filed March 9, 2023. [Background technology]

[0002] FIELD OF THE DISCLOSURE The present disclosure relates generally to precursor ampoules, and more particularly to multi-chamber solid precursor ampoules.

[0003] A solid-phase precursor for delivering precursor vapors for vapor-based applications such as semiconductor manufacturing and fabrication. A carrier gas is supplied to an ampoule containing the solid precursor, where the solid precursor vaporizes through a sublimation process to produce precursor vapor. To ensure consistent delivery of the precursor vapor, the atmospheric conditions inside the ampoule, as well as the headspace pressure and temperature, are carefully controlled.

[0004] The physical phenomena occurring within a solid-source sublimation ampoule are a complex, multiphysics problem, combining fluid dynamics, heat transfer, and mass transfer. The flow and thermal properties of the ampoule affect mass transfer, and these effects are closely coupled and mutually influential. Changing the flow properties of the ampoule can alter the distribution of mass transfer locations and therefore the heat load driving the required thermal properties. Changing the thermal properties of the ampoule can alter the distribution of vapor pressure across the sublimation surface, affecting the concentration gradient and mass transfer to the carrier gas stream. Therefore, the flow and thermal properties of the ampoule are considered in parallel. Therefore, ampoule design must ensure that regions of the ampoule with favorable flow properties are matched with favorable thermal properties.

[0005] Thermal properties must ensure that the ampoule allows sufficient heat transfer to the precursor surface to prevent significant surface cooling from the latent heat extracted during sublimation. The highest heat flux is found in the area with the highest mass transfer. If the ampoule cannot provide sufficient heat transfer, the temperature drop at the sublimation surface will be large, thereby reducing the sublimation rate. The vapor pressure of the precursor is typically described by the Antoine equation, which has an exponential relationship between vapor pressure and temperature. Therefore, a small decrease in temperature results in a large decrease in vapor pressure, reducing the mass transfer rate. Therefore, the thermal properties of the ampoule must ensure that a high heat transfer rate is possible between the heat source and the area of ​​highest mass transfer. Generally, the materials of construction of the ampoule have a much higher thermal conductivity than the precursor itself. Precursors in contact with or close to the walls of the ampoule generally maintain a higher temperature than precursors away from the walls. Because the heat source is typically in communication with the exterior surface of the ampoule, the thermal property issue involves conducting heat from the outside of the ampoule to the surface of the precursor with the highest flux rate.

[0006] A single large bulk chamber filled with precursor has poor thermal properties because any material that sublimes from the walls must be conducted through a large path length of low thermal conductivity precursor, resulting in a large temperature drop at the center of the vessel. To solve this problem, prior art sublimation ampoules may utilize trays, fins, or other protrusions to increase the ratio of precursor surface area in contact with the high thermal conductivity material to precursor volume.

[0007] The problem of solid source precursor delivery is further complicated by the consistency of delivery rate over the life of the ampoule: prior art solid source delivery systems provide adequate initial delivery rate performance, but as the precursor is depleted, the delivery rate decreases, which requires complex adjustments to the flow and thermal properties of the system.

[0008] For example, as the solid precursor depletes more quickly from certain areas, it can alter the way the carrier gas flows through the ampoule, thereby changing its flow characteristics. This can also result in a change in the heat conduction path to the sublimation surface, due to the ampoule walls conducting heat better than the center of the ampoule. When the precursor is initially in contact with the container walls, these areas are hottest, facilitating mass transfer. Once enough material sublimes and loses contact with the container walls, heat is no longer conducted directly to the surface. Heat must be convected or radiated across the gap, which is negligible under vacuum process conditions and relatively small temperature differences. Otherwise, heat must be conducted a much longer distance to the precursor surface, such as from the bottom of the container to the precursor surface. When this occurs, a larger temperature gradient is created than if heat were conducted directly from the container walls. Low surface temperatures can affect mass transfer, alter delivery rates, and disrupt customer deposition processes.

[0009] Therefore, the design of a solid source ampoule must carefully consider the balance of all three transport phenomena: flow, heat transfer, and mass transfer. Each of these has two-way coupling that influences the others. All of these factors must be carefully weighed by the designer to provide optimal performance. This is not only to provide complete carrier gas saturation upon initial installation, but also to ensure that carrier gas saturation remains constant throughout the life of the ampoule. With the secondary goal of achieving maximum saturation, it is desirable to provide a consistent delivery rate throughout the life of the ampoule.

[0010] Prior art systems utilizing trays, fins, or other protrusions to facilitate sublimation are difficult to disassemble, reassemble, clean, and refill. For example, each tray must be individually removed for cleaning, often with numerous nooks and crannies that are difficult to remove from precursor residue. Conversely, when filling a container, the trays must be individually loaded and assembled in an inert environment, such as a glove box. Such complex cleaning and refilling processes result in longer downtime and tooling. Furthermore, complex ampoule configurations with complex interiors hinder cleaning and filling operations, while they occupy valuable volume inside the container that could otherwise be filled with solid precursor.

[0011] Therefore, there is a need to improve the flow and thermal properties of solid precursor ampoules. Summary of the Invention

[0012] In one aspect of the present disclosure, a sublimation ampoule is disclosed. The ampoule includes a sublimation container and a container lid. The sublimation container has an open end, a closed end, a sidewall, and at least two chambers extending between the open end and the closed end. Each chamber is separated by a container wall, and each chamber has a surface area and a sublimation rate. The container lid has a top surface and a bottom surface that define a thickness. The bottom surface is removably securable to the open end of the sublimation container to form a fluid seal.

[0013] The container lid further includes a lid inlet disposed on a top surface of the container lid, the lid inlet extending through the thickness. The container lid further includes a lid outlet disposed on the top surface of the container lid, the lid outlet extending through the thickness. The container lid further includes at least one chamber inlet disposed on a bottom surface of the container lid fluidly connected to the lid inlet. Each chamber inlet is fluidly connected to one of the at least two chambers, each chamber inlet having a cross-sectional area. The container lid further includes a conduit having a conduit inlet and a conduit outlet disposed on the bottom surface. The conduit inlet and the conduit outlet extend partially through the thickness, and the conduit fluidly connects to two of the at least two chambers. The conduit has a cross-sectional area. The sublimation rate of each chamber is determined by the surface area of ​​each chamber, the temperature of each chamber, and the headspace pressure of each chamber, and the sublimation rate of each chamber is substantially equal.

[0014] In another aspect of the present disclosure, a sublimation ampoule is disclosed. The sublimation ampoule comprises a sublimation container and a sublimation lid. The sublimation container has an open end and a closed end, a sidewall, and a central longitudinal axis. The sublimation container includes an inner wall extending across the sidewall of the sublimation container, a radial wall concentric with the central longitudinal axis, a first chamber and a second chamber separated by the inner wall, and a third chamber and a fourth chamber separated from the first chamber and the second chamber by the radial wall and adjacent to the sidewall of the sublimation container. The container lid has a top surface and a bottom surface defining a thickness. The bottom surface is removably securable to the open end of the sublimation container to form a fluid seal. The container lid includes: a lid inlet located on the top surface of the container lid and having a fixed inlet flow rate, the lid inlet extending through the thickness; at least one chamber inlet located on the bottom surface of the container lid fluidly connected to the lid inlet, the chamber inlet fluidly communicating with the first chamber and having a cross-sectional area; and a lid outlet located on the top surface of the container lid and having a fixed outlet pressure, the lid outlet extending through the thickness and fluidly communicating with the fourth chamber. The container lid further includes a plurality of conduits having a conduit inlet and a conduit outlet located on the bottom surface, the conduit inlet and the conduit outlet extending partially within the thickness, the conduits fluidly connecting the first chamber, the second chamber, the third chamber, and the fourth chamber, each of the plurality of conduits having a cross-sectional area. The sublimation rate of each chamber is determined by the surface area of ​​each chamber, the temperature of each chamber, and the headspace pressure of each chamber, and the sublimation rates of each chamber are substantially equal. [Brief explanation of the drawings]

[0015] The subject matter of the invention will be explained in more detail in the following text with reference to exemplary embodiments shown in the accompanying drawings.

[0016] [Figure 1] FIG. 1 illustrates a perspective view of an exemplary sublimation ampoule according to one or more embodiments of the present disclosure. [Figure 2] 2 shows a cross-sectional view of the sublimation ampoule of FIG. 1 taken along the line X-X'. [Figure 3] 2 shows an exploded view of the sublimation ampoule of FIG. 1. [Figure 4]2 shows a top view of the sublimation ampoule container of FIG. 1. [Figure 5] 2 shows a top view of the sublimation ampoule lid of FIG. 1 positioned on a container. [Figure 6A] 2 shows a cross-sectional schematic view of the sublimation ampoule of FIG. 1 along section line X-X′, with emphasis on the configuration of the lid. [Figure 6B] 2 shows a cross-sectional schematic view of the sublimation ampoule of FIG. 1 along section line X-X′, with emphasis on the configuration of the lid. [Figure 6C] 2 shows a cross-sectional schematic view of the sublimation ampoule of FIG. 1 along section line X-X′, with emphasis on the configuration of the lid. [Figure 6D] 2 shows a cross-sectional schematic view of the sublimation ampoule of FIG. 1 along section line X-X′, with emphasis on the configuration of the lid. [Figure 7A] 1 shows an ampoule with two chambers having the same surface area. [Figure 7B] 1 shows an ampoule with three chambers. [Figure 7C] 1 shows an ampoule with four chambers. [Figure 8] 1 shows an ampoule having two chambers of unequal surface area. [Figure 9A] 1 shows an ampoule with two chambers having the same surface area. [Figure 9B] 1 shows an ampoule with three chambers having the same surface area. [Figure 10] 1 shows an ampoule with two chambers having the same surface area. [Figure 11] 1 shows a two-chambered ampoule having a first chamber and a second chamber separated by a radial wall. [Figure 12] 1 shows an ampoule having an interior wall that separates the container into two halves and radial walls that further separate the container and define four chambers. [Figure 13] 1 shows an ampoule having two interior walls that separate the container into four halves and radial walls that further separate the container into eight chambers. [Figure 14]1 illustrates a precursor delivery system according to one or more embodiments of the present disclosure.

[0017] The reference signs used in the drawings and their meanings are summarized in the list of reference signs. As a rule, identical parts in the drawings are provided with the same reference signs. DETAILED DESCRIPTION OF THE INVENTION

[0018] In the following specification and claims, reference will be made to a number of terms that shall be defined to have the following meanings.

[0019] As used herein, the singular forms "a," "an," and "the" include plural references unless the context dictates otherwise. The terms "comprising," "including," and "having" are intended to be inclusive and mean that there may be additional elements other than the listed elements. The term "optional" or "optionally" means that the subsequently described event or circumstance may or may not occur, and that the description includes instances where the event occurs or does not occur.

[0020] Unless otherwise specified, approximating language such as "generally," "substantially," and "about" used herein indicates that the modified term may apply only to an approximate degree, and not to an absolute or complete degree, as would be recognized by one of ordinary skill in the art. Thus, values ​​modified by terms such as "about," "approximately," and "substantially" are not limited to the exact value specified. In at least some instances, approximating language may correspond to the precision of an instrument for measuring the value. Herein, range limitations may be specified throughout the specification and claims. Such ranges may be combined and / or interchangeable, and include all subranges contained therein, unless the context or language indicates otherwise.

[0021] Further, unless otherwise stated, terms such as "first," "second," and the like are used herein merely as labels, and are not intended to impose any order, position, or hierarchy on the items to which these terms refer. Further, for example, a reference to a "second" item does not require or preclude the presence of, for example, a "first" or lower-numbered item, or a "third" or higher-numbered item.

[0022]

[0003] Embodiments of the present disclosure are directed to a multi-chamber sublimation ampoule including a sublimation container and a container lid. The container has an open end, a closed end, and a sidewall defining at least two chambers extending between the open and closed ends. Each chamber is separated by a container wall, and each chamber has a surface area and a sublimation rate. The container lid has a top surface and a bottom surface defining a thickness, and the bottom surface is removably securable to the open end of the sublimation container to form a fluid seal.

[0023] The container lid further includes a lid inlet disposed on a top surface of the container lid, a lid outlet disposed on the top surface of the container lid and extending through the thickness, and at least one chamber inlet disposed on a bottom surface of the container lid fluidly connected to the lid inlet, each chamber inlet fluidly connected to one of the at least two chambers, each chamber inlet having a cross-sectional area. The container lid further includes a conduit having a conduit inlet and a conduit outlet disposed on the bottom surface. The conduit inlet and conduit outlet extend partially through the thickness, the conduit fluidly connected to two of the at least two chambers, the conduit having a cross-sectional area.

[0024] Carrier gas is supplied to the ampoule through the lid inlet and, as the carrier gas passes from the lid conduit between the chambers, it gradually becomes saturated with vaporized precursor through a sublimation process. The sublimation rate of each chamber is determined by the relative surface area of ​​each chamber, the relative temperature gradient of each chamber, and the headspace pressure of each chamber (which is a function of the transfer restriction between the chambers). The present disclosure enables each chamber to have a substantially equal sublimation rate so that each chamber is completely depleted over the lifetime (operation) of the sublimation ampoule. As used herein, the term "sublimation rate" refers to a measurement of the amount of solid precursor sublimed (depleted) from a chamber as a function of time, and is expressed in SI units as mg / min / cm. 2 It is measured in terms of mass sublimated over time relative to surface area. This disclosure also considers the volume of solid precursor in each chamber, and for purposes of this disclosure, each chamber is filled to the same level.

[0025] It is understood that the sublimation rates (as a function of the relative surface area of ​​each chamber, the relative temperature gradient of each chamber, and the headspace pressure of each chamber) will result in a uniform sublimation rate under ideal conditions. However, as previously mentioned, the sublimation process is a complex, coupled, multiphysics problem of fluid dynamics, heat transfer, and mass transfer, and secondary factors can affect the sublimation rate of each chamber. In practice, the sublimation rate may therefore be slightly non-uniform due to secondary factors outside the scope of this disclosure. If sublimation is unequal due to external factors (resulting in up to 20% solid precursor remaining in the chamber), less solid precursor material can be loaded into chambers that might otherwise not be fully depleted, resulting in the entire ampoule being fully depleted nonetheless. In other words, to achieve equal sublimation rates under non-ideal conditions, the difference between chambers can be corrected by adding less precursor material to those chambers. Ideal conditions are calculated and optimized by computer-aided simulation and finite element analysis. Actual (non-ideal) conditions are observed and determined through prototype and pilot testing.

[0026] 1-5 illustrate an exemplary multi-chamber sublimation ampoule 100 (hereinafter referred to as ampoule 100) according to one or more embodiments of the present disclosure. FIG. 1 is a perspective view. FIG. 2 illustrates a cross-sectional view of FIG. 1 along section line X-X', and FIG. 3 illustrates an exploded view of ampoule 100. Ampoule 100 includes a multi-chamber sublimation container 110 (hereinafter referred to as container 110) and a container lid 160 (hereinafter referred to as lid 160). FIG. 4 illustrates a top view of container 110, and FIG. 5 illustrates a top view of lid 160 disposed on container 110.

[0027] The container 110 includes an open end 112, a closed end 114, and a sidewall 116 that defines an interior cavity 118 of the container 110. In some embodiments, the open end 112 includes a flange 120 for securing or fastening the container 110 to a lid 160. In some embodiments, the closed end 114 and the sidewall 116 define a unitary cylindrical body. In some embodiments, the closed end 114 is fastened to the sidewall 116 such that the closed end 114 can be removed from the sidewall 116 for cleaning and refilling the interior cavity 118. To facilitate heating of the sidewall 116 of the sublimation container 110, side heaters 102 are disposed around the ampoule 100 and a bottom heater 104 is disposed adjacent the closed end 114. In some embodiments, the opening 106 extends a distance within the container 110 from the closed end 114. A cartridge heater 108 may be positioned within the opening 106 to internally heat the vessel 110. The heat output of the side heater 102, bottom heater 104, and cartridge heater 108 may be increased or decreased in response to changes in mass flow and fluid flow characteristics during the sublimation process.

[0028] The container 110 includes at least two chambers 130 extending between an open end 112 and a closed end 114. The at least two chambers 130 are separated by a container wall 122 disposed within the cavity 118, and each of the at least chambers 130 has a surface area. This surface area is relative to and parallel to the open end 112. Because the sidewall 116 and the container wall 122 are perpendicular to the open end 112, the surface area is consistent for each chamber between the open end 112 and the closed end 114. The sublimation rate of each of the at least two chambers 130 depends (for purposes of this disclosure) on the relative surface area of ​​each chamber, the relative temperature gradient of each chamber, and the headspace pressure of each chamber.

[0029] The terms “at least two chambers,” “plurality of chambers,” “two or more chambers,” and “chamber” are generally used interchangeably and are designated by the reference numeral “130.” As used herein, one of the at least two chambers 130 is designated by the reference numeral “130-n,” where “n” indicates an integer corresponding to one of the at least two chambers. Thus, the first chamber is “130-1,” the second chamber is “130-2,” and the nth chamber is “130-n.” The first chamber 130-1 is in fluid communication with the inlet 166 of the lid 160. The second chamber 130-2 is in fluid communication with the first chamber 130-1 by one or more conduits 172 of the lid 160, and the nth chamber 130-n (the last chamber) is in fluid communication with the outlet 168 of the lid 160. The nth chamber is downstream of the first chamber, and the intermediate chamber is between the first chamber and the nth chamber.

[0030] As described in more detail below, the chambers 130 may be in a series or parallel configuration with respect to the carrier gas entering or exiting the chambers, and thus in some embodiments, the first two chambers (130-1, 130-2) may both be in parallel fluid communication with the inlet 166 of the lid 160. Similarly, any two or more chambers 130 may be in fluid communication with a single conduit 172 or with the outlet 168 of the lid 160.

[0031] The lid 160 includes a top surface 162 and a bottom surface 164 that define a thickness. The bottom surface 164 is removably securable to the open end 112 (and flange 120) of the container 110 to form a fluid seal. The lid 160 further includes a lid inlet 166 disposed on the top surface 162 of the lid 160 and a lid outlet 168 disposed on the top surface 162 of the lid 160. The lid inlet 166 and the lid outlet 168 extend through the thickness of the lid 160 to facilitate fluid connection of the ampoule 100 to a precursor delivery system (not shown). The lid inlet 166 is in fluid communication with at least one chamber inlet 170 disposed on the bottom surface 164 of the lid 160, with each chamber inlet 170 fluidly connected to one of the at least two chambers 130 of the container 110.

[0032] Carrier gas is supplied to the lid inlet 166, distributed to at least one chamber inlet 170, and distributed into a corresponding one of the at least two chambers 130. Generally, each chamber inlet 170 has a cross-sectional area that defines the headspace pressure of each chamber inlet 170 (among other parameters, including the pressure of the carrier gas supplied to the lid inlet 166). In some embodiments, the lid inlet 166 is fluidly connected to a single chamber inlet 170. In some embodiments, the lid inlet 166 is connected to at least two chamber inlets 170 in a parallel configuration. Generally, the cross-sectional areas of the at least two chamber inlets 170 are equal, resulting in equal distribution of the carrier gas from the lid inlet 166.

[0033] The lid 160 further includes a plurality of conduits 172 extending through the thickness of the lid 160 to connect the chambers 130 to one another. Each conduit 172 includes at least one conduit inlet 174 and at least one conduit outlet 176 disposed on the bottom surface 164. The conduit inlets 174 and the conduit outlets 176 extend partially through the thickness of the lid 160 to facilitate connections between the chambers 130.

[0034] 4, the vessel wall 122 can include radial walls 124 and inner walls 126 to subdivide the vessel 110 into chambers 130. In the illustrated embodiment, the radial walls 124 are concentric with the longitudinal axis A-A' (also shown in FIG. 2), and the inner walls 126 extend through the longitudinal axis A-A' and contact the side walls 116 of the vessel 110 on opposite sides within the interior cavity 118. The radial walls 124 and the inner walls 126 are made from a thermally conductive material that facilitates heat transfer from the side heaters 102 (of FIG. 1) to the interior of the vessel 110.

[0035] As will be explained in more detail below, the chamber 130 adjacent the sidewall 116 of the vessel 110 is heated to a higher temperature than the chamber 130 within the radial wall 124. Thus, the chambers 130 adjacent the sidewall 116 of the vessel 110 have a substantially equal temperature gradient.

[0036] By utilizing multiple chambers 130 within a single vessel 110 and connecting them in series or parallel via conduits 172 in the lid 160, potential cooling effects within upstream or adjacent chambers 130 are isolated from subsequent chambers 130, resulting in better thermal characteristics for the subsequent chambers 130. Because the carrier gas is reheated as it travels through the lid 160 between chambers 130, subsequent chambers also experience improved thermal characteristics. Furthermore, by directing the carrier gas at the surfaces of the multiple chambers 130, sufficient surface area is achieved for full carrier gas saturation. Flow into each chamber is directed downward at the surface area of ​​the solid precursor to provide good flow characteristics. Furthermore, flow into each chamber 130 is directed to the location of the surface to balance these two characteristics, ensuring that sublimation occurs uniformly across the surface and remains largely constant over time.

[0037] In many ampoule heating applications, the lid is maintained at a higher temperature than the base to prevent condensation from occurring on the lid. Therefore, routing the carrier gas between chambers through the lid allows for the ability to superheat the carrier gas to higher temperatures than would be possible with a carrier gas routed between chambers through the lid. The reheated carrier gas brings more energy to the sublimation surface, enhancing sublimation in the latter chamber, where sublimation would otherwise be less likely. The precursor vapor typically has a higher specific heat capacity than the carrier gas. When traveling between chambers, the carrier gas picks up some precursor vapor from the first chamber(s), resulting in a mixture with a higher heat capacity than the carrier gas, further enhancing heat transfer to the sublimation surface in the subsequent chamber.

[0038] As shown in FIG. 5 , carrier gas is supplied into ampoule 100 through inlet 166. The path the carrier gas takes between chambers is indicated by dashed arrows. In this exemplary embodiment, all chambers (130-1 through 130-15) are connected in series via conduit 172, with the first chamber 130-1 receiving carrier gas from inlet 166 and the fifteenth chamber 130-15 receiving carrier gas from the upstream fourteenth chamber 130-14. As the carrier gas passes through each chamber (130-1 through 130-15), it becomes increasingly saturated with vaporized precursor, causing the solid precursor to sublimate. The fully saturated carrier gas exits fifteenth chamber 130-15 through outlet 168. The embodiment shown in FIG. 5 is merely an exemplary diagram of ampoule 100 and is not intended to be limiting.

[0039] 6A-6D show schematic cross-sectional views of ampoule 100 along section line X-X', with emphasis on the configuration of lid 160. As shown in FIG. 6A, lid inlet 166 is disposed on top surface 162 of lid 160, and lid outlet 168 is disposed on top surface 162 of lid 160. Lid inlet 166 and lid outlet 168 extend through the thickness of lid 160, with lid inlet 166 in fluid communication with one chamber inlet 170. Conduit 172 extends across the thickness, and both conduit inlet 174 and conduit outlet 176 extend into the thickness to facilitate fluid communication between the serially configured chambers (130-1, 130-2). In the configuration of FIG. 1, carrier gas is supplied to first chamber 130-1, and the carrier gas then enters second chamber 130-2. The carrier gas then exits ampoule 100 via lid outlet 168.

[0040] As shown in FIG. 6B, the lid inlet 166 is in fluid communication with two chamber inlets 170, each of which is in fluid communication with a first chamber 130-1 and a second chamber 130-2 that define a parallel configuration. Both the first chamber 130-1 and the second chamber 130-2 are fluidly connected to a third chamber 130-3 by a conduit 172. In the illustrated embodiment, the carrier gas exits the third chamber 130-3 by a lid outlet 168. Because FIG. 6B is shown in two dimensions, the fluid connection between the first chamber 130-1 and the third chamber 130-3 is not shown.

[0041] 6C, the lid inlet 166 is in fluid communication with one chamber inlet 170, and the conduit 172 includes two conduit outlets 176. The lid inlet 166 to one chamber inlet 170 defines a series configuration, and the conduit 172 with two conduit outlets 176 defines a parallel configuration.

[0042] 6D , the lid inlet 166 is in fluid communication with two chamber inlets 170, and the conduit 172 includes two conduit outlets 176, defining a series configuration. In some embodiments, the lid inlet 166 can be connected to at least two chamber inlets 170. In some embodiments, the conduit 172 includes at least two conduit outlets 176.

[0043] Generally, each conduit 172 has a cross-sectional area that defines the headspace pressure of the corresponding chamber. Therefore, the headspace pressure is a function of the cross-sectional area of ​​the conduit 172 and the headspace pressure from the upstream chamber 130. In some embodiments, the conduit outlet 176 can include a provision for a fixture or showerhead to selectively adjust the flow characteristics of the carrier gas passing through the conduit outlet 176. A showerhead is a device for uniformly distributing gas over a larger surface area. The showerhead includes an inlet fixture removably connected to the conduit outlet 176 and a perforated outlet having a larger surface area than the showerhead inlet. It should be understood that the headspace pressure of any of the chambers 130 is affected, directly or indirectly, by the cross-sectional area of ​​the chamber inlet 170 and the cross-sectional area of ​​the downstream conduit 172. For purposes of this disclosure, the parameters that affect the headspace pressure of any given chamber are referred to as the “transfer constraints” between chambers 130.

[0044] 7A-7C, 8, and 9 show top views of an embodiment of ampoule 100 in which sublimation rates between chambers 130 are substantially equal by adjusting one or more of the following parameters: (1) changing the travel restrictions between chambers 130; (2) adjusting the relative surface areas of chambers 130; and (3) by relative temperature gradients between chambers 130. As explained in more detail below, the arrangement of chambers in a series or parallel configuration also affects the sublimation rate. Finally, further subdivision of container 110 into additional chambers 130 also affects the sublimation rate. Ampoule 100 can have any number of chambers 130, facilitated by the illustrated configuration of radial walls 124 and interior wall 126.

[0045] In general, movement restrictions between chambers can be modified by increasing or decreasing the cross-sectional area of ​​the conduits 172, adding additional conduits 172 between chambers 130 so that the chambers 130 have a side-by-side configuration, and using fixtures and showerheads to the conduit outlets 176 and / or lid inlets 166. Adjusting the relative surface area between chambers 130 is determined by the configuration of the radial walls 124 and inner walls 126. The relative temperature gradients in the chambers 130 are determined by the proximity of the chamber placement of the chambers 130 to the sidewalls 116 and side heaters 102 (as shown in FIG. 1 ).

[0046] 7A shows ampoule 100 having two chambers (130-1, 130-2) with the same surface area and therefore the same volume. First chamber 130-1 and second chamber 130-2 are separated by interior wall 126 so that first chamber 130-1 and second chamber 130-2 have the same surface area. First chamber 130-1 is in a series configuration with second chamber 130-2 by a single conduit 172 connecting the two chambers (130-1, 130-2).

[0047] Because both chambers (130-1, 130-2) are adjacent to the sidewall 116, both chambers (130-1, 130-2) have the same temperature gradient. To equalize the sublimation rates between the chambers (130-1, 130-2), the transport restriction between the chambers (130-1, 130-2) is increased, thereby lowering the sublimation flux in the first chamber 130-1 to match that of the second chamber 130-2. In general, increasing the transport restriction increases the pressure in the upstream chamber 130, which limits mass transport within the upstream chamber 130. The first chamber 130-1 has a high degree of saturation due to the headspace pressure from the lid inlet 166, but the degree of saturation is reduced due to the headspace pressure downstream from the first chamber 130-1. Thus, the restriction to saturation in the first chamber 130-1 results in a reduction in mass transfer to balance the chambers (130-1, 130-2). To reduce the transfer restriction between the chambers (130-1, 130-2), the cross-sectional area of ​​the conduit 172 can be made smaller or a restriction fitting can be added to the conduit outlet 176.

[0048] The same concept can be applied to multiple chambers 130 connected in series. Figure 7B shows an ampoule 100 with three chambers (130-1, 130-2, 130-3). Figure 7C shows an ampoule 100 with four chambers (130-1, 130-2, 130-3, 130-4). For both of the embodiments shown in Figures 7B and 7C, the interior wall 126 subdivides the chambers 130 into equal surface areas, and each of the chambers 130 has the same volume. Adjacent chambers 130 are connected in series by a single conduit 172 between the chambers 130. Because the chambers 130 are all adjacent to the side wall 116, the chambers 130 have the same temperature gradient.

[0049] The first chamber 130-1 has the highest sublimation rate due to the highest gas concentration gradient from the lid inlet 166. To limit saturation in the first chamber 130-1 and equalize the sublimation rate with the downstream chambers 130, the transport restrictions of the downstream chambers can be gradually increased. To reduce the transport restrictions between the downstream chambers 130, the cross-sectional area of ​​the conduit 172 can be made smaller, or a restriction fitting can be added to the conduit outlet 176. Thus, the conduit 172 between the first chamber 130-1 and the second chamber 130-2 has a larger cross-sectional area than the conduit 172 between the second chamber 130-2 and the third chamber 130-3. This configuration can be scaled to any number of additional chambers 130 with the same surface area. Experimental data has shown that the above configuration is effective for up to 16 chambers.

[0050] 8 shows an ampoule 100 having two chambers (130-1, 130-2) with unequal surface areas and therefore unequal volumes. The first chamber 130-1 and the second chamber 130-2 are separated by an interior wall 126 such that the first chamber 130-1 has a larger surface area than the second chamber 130-2. The first chamber 130-1 is in series with the second chamber 130-2 by a single conduit 172 connecting the two chambers (130-1, 130-2). Because both chambers (130-1, 130-2) are adjacent to the sidewall 116, both chambers (130-1, 130-2) have the same temperature gradient.

[0051] To equalize the sublimation rates between the chambers (130-1, 130-2), the relative surface areas of the chambers (130-1, 130-2) are adjusted so that the sublimation flux of the second chamber 130-2 is greater than that of the first chamber 130-1. This configuration compensates for the upstream chamber having most of its sublimation occurring and being depleted before the downstream chamber.

[0052] 9A shows ampoule 100 having two chambers (130-1, 130-2) having the same surface area and therefore the same volume. First chamber 130-1 and second chamber 130-2 are separated by interior wall 126 so that first chamber 130-1 and second chamber 130-2 have the same surface area. First chamber 130-1 is in a series configuration with second chamber 130-2 by two parallel conduits 172 connecting the two chambers (130-1, 130-2).

[0053] Because both chambers (130-1, 130-2) are adjacent to the sidewall 116, both chambers (130-1, 130-2) have the same temperature gradient. To equalize the sublimation rates between the chambers (130-1, 130-2), the transport restriction between the chambers (130-1, 130-2) is increased, thereby lowering the sublimation flux in the first chamber 130-1 to match that of the second chamber 130-2. Having multiple parallel conduits 172 reduces the standard deviation of the sublimation flux by distributing the carrier gas more uniformly across the chamber surfaces. This concept can also be combined with various transport restrictions between the conduits 172, similar to the embodiment of FIG. 7A, where the transport restriction between the chambers (130-1, 130-2) is reduced (by reducing the cross-sectional area of ​​the conduits 172).

[0054] 9B shows ampoule 100 having three chambers (130-1, 130-2, 130-3) with the same surface area and therefore the same volume. Chambers 130-1, 130-2, 130-3 are separated by interior wall 126. Inlet 166 includes two chamber inlets 170 such that first chamber 130-1 and second chamber 130-2 are in a parallel configuration relative to inlet 166. Each of first chamber 130-1 and second chamber 130-2 is connected to third chamber 130-3 by conduit 172. Because chambers 130-1, 130-2, 130-3 are adjacent sidewall 116, chambers 130-1, 130-2, 130-3 have the same temperature gradient.

[0055] This embodiment combines the concept of multiple chambers as shown in Figures 7B and 7C with the concept of the parallel configuration of chambers of Figure 9A. In particular, the first chamber 130-1 and the second chamber 130-2 have the highest sublimation rates due to the highest gas concentration gradient from the lid inlet 166, and saturation of the first chamber 130-1 and the second chamber 130-2 is limited by restricting the size of the conduit 172 to the third chamber 130-3. The parallel configuration helps reduce the standard deviation of the sublimation flux.

[0056] Therefore, to equalize the sublimation rate between the chambers (130-1, 130-2, 130-3), the transfer restriction between the first chamber 130-1 and the second chamber 130-2 to the third chamber 130-3 is increased. Having multiple parallel conduits 172 reduces the standard deviation of the sublimation flux by distributing the carrier gas more evenly across the chamber surfaces.

[0057] 10 shows an ampoule 100 having two chambers (130-1, 130-2) having the same surface area and therefore the same volume. The first chamber 130-1 and the second chamber 130-2 are separated by an interior wall 126 so that the first chamber 130-1 and the second chamber 130-2 have the same surface area. The first chamber 130-1 is in a series configuration with the second chamber 130-2 by a conduit structure 200 that connects the two chambers (130-1, 130-2).

[0058] This embodiment illustrates the use of a showerhead configuration for at least one of the inlet 166 and the conduit structure 200. In some embodiments, the lid 160 includes multiple chamber outlets 167 that distribute the carrier gas evenly within the first chamber 130-1. In some embodiments, the conduit structure 200 includes multiple conduit outlets 202 that distribute the carrier gas evenly within the second chamber 130-2. The distribution of the carrier gas as a result of the showerhead configuration promotes greater distribution uniformity of the carrier gas.

[0059] Because both chambers (130-1, 130-2) are adjacent to the sidewall 116, both chambers (130-1, 130-2) have the same temperature gradient. To equalize the sublimation rates between the chambers (130-1, 130-2), the transport restriction between the chambers (130-1, 130-2) is increased, thereby lowering the sublimation flux in the first chamber 130-1 to match that of the second chamber 130-2. Having multiple parallel conduits 172 reduces the standard deviation of the sublimation flux by distributing the carrier gas more evenly across the surfaces of the chambers.

[0060] FIG. 11 shows ampoule 100 having two chambers (130-1, 130-2), with first chamber 130-1 and second chamber 130-2 separated by radial wall 124. Second chamber 130-2 is adjacent to sidewall 116 and therefore has a higher temperature gradient relative to first chamber 130-1. In some embodiments, first chamber 130-1 and second chamber 130-2 have equal surface areas and therefore the same volume. In some embodiments, first chamber 130-1 and second chamber 130-2 have unequal surface areas. In some embodiments, first chamber 130-1 and second chamber 130-1 are connected in series with a single conduit 172. In some embodiments, first chamber 130-1 and second chamber 130-1 are connected in parallel with multiple conduits 172.

[0061] The sublimation rate of the first chamber 130-1 is increased due to the first chamber 130-1 being upstream of the second chamber 130-2 (similar to the embodiment of FIG. 7A), and the sublimation rate of the second chamber 130-2 is increased due to the second chamber 130-2 having a higher temperature gradient.

[0062] In some embodiments, the sublimation rate is equalized by increasing the travel restriction of the second chamber 130-2. In some embodiments, the sublimation rate is equalized by increasing the surface area of ​​the second chamber 130-2. In some embodiments, the sublimation rate is equalized by a combination of increasing the travel restriction of the second chamber 130-2 and increasing the surface area of ​​the second chamber 130-2. These concepts can be combined for a more optimal ampoule configuration 100, as shown in FIGS. 12 and 13.

[0063] 12 shows ampoule 100 having an interior wall 126 that separates container 110 into two halves and radial walls 124 that further separate container 110 to define four chambers (130-1, 130-2, 130-3, 130-4). First chamber 130-1 and second chamber 130-2 are internal to third chamber 130-3 and fourth chamber 130-4.

[0064] The third chamber 130-3 and the fourth chamber 130-4 are adjacent to the sidewall 116 and therefore have a higher temperature gradient relative to the first chamber 130-1 and the second chamber 130-2. In the illustrated embodiment, the first chamber 130-1 and the second chamber 130-2 have the same surface area. The third chamber 130-3 and the fourth chamber 130-4 have the same area. In some embodiments, the chambers (130-1, 130-2, 130-3, 130-4) have equal surface areas and therefore have the same volume. In some embodiments, the chambers (130-1, 130-2, 130-3, 130-4) have unequal surface areas.

[0065] In the illustrated embodiment, the surface areas of the first chamber 130-1 and the second chamber 130-2 are smaller than the surface areas of the third chamber 130-3 and the fourth chamber 130-4. Similar to the embodiment of Figure 8, the surface areas of the third chamber 130-3 and the fourth chamber 130-4 are larger than the surface areas of the first chamber 130-1 and the second chamber 130-2, thereby equalizing, or at least partially equalizing, the sublimation rates of the third chamber 130-3 and the fourth chamber 130-4 relative to the first chamber 130-1 and the second chamber 130-2.

[0066] The sublimation rates of the chambers (130-1, 130-2, 130-3, 130-4) are further equalized by the third chamber 130-3 and the fourth chamber 130-4 having a larger temperature gradient relative to the first chamber 130-1 and the second chamber 130-2, similar to the embodiment of FIG. 11.

[0067] Since the upstream chambers (first chamber 130-1 and second chamber 130-2) have a higher sublimation rate compared to the downstream chambers (third chambers 130-3 and 130-4), the movement restriction of the downstream chambers (130-3, 130-4) can be increased by reducing the cross-sectional area of ​​the conduit 172 connecting the chambers, similar to the embodiment of FIG. 7A.

[0068] In some embodiments, the chambers (130-1, 130-2, 130-3, 130-4) are connected in series with a single conduit 172 between the chambers. In some embodiments, the chambers (130-1, 130-2, 130-3, 130-4) are connected in parallel with two or more conduits 172 between the chambers. In some embodiments, a combination of a single conduit 172 and multiple conduits 172 can be used to facilitate the series and parallel connections.

[0069] Thus, the sublimation rate can be equalized by changing the relative temperature gradients of the chambers 130 by changing the travel restrictions between the chambers 130 and adjusting the relative surface areas of the chambers 130. Furthermore, arranging the chambers in a series or parallel configuration also facilitates equalization of the sublimation rate. Finally, further subdividing the vessel 110 into additional chambers 130 also affects the sublimation rate, as shown in FIG. 13.

[0070] 13 shows an ampoule having two interior walls 126 that separate the container 110 into four halves and radial walls 124 that further separate the container 110 into eight chambers (130-1, 130-2, 130-3, 130-4, 130-5, 130-6, 130-7, 130-8). The first chamber 130-1, the second chamber 130-2, the third chamber 130-3, and the fourth chamber 130-4 are internal to the fifth chamber 130-5, the sixth chamber 130-6, the seventh chamber 130-7, and the eighth chamber 130-8. Therefore, the fifth chamber 130-5, the sixth chamber 130-6, the seventh chamber 130-7, and the eighth chamber 130-8 have a higher temperature gradient than the first chamber 130-1, the second chamber 130-2, the third chamber 130-3, and the fourth chamber 130-4 because they are closer to the sidewall 116.

[0071] Figure 14 shows a precursor delivery system 300 that includes the ampoule 100 of Figures 1-13. The system includes a carrier gas supply 302 that delivers a carrier gas to the ampoule 100, and a carrier gas outlet supply 304. The system 300 regulates the concentration of the carrier gas and the flow rate of the carrier gas from the gas supply 302 so that the saturated carrier gas exiting the gas outlet supply 304 has a constant outlet flow rate and a constant degree of saturation. To achieve sublimation within the ampoule 100, the system also regulates the temperature of the ampoule 100 by operation of a side heater 102.

[0072] Ampoule 100 is shown schematically and includes at least three chambers (130-1, 130-2, 130-3). Inlet 166 can be connected to first chamber 130-1 by at least one chamber inlet 170 in a series configuration. Alternatively, inlet 166 can be connected to first chamber 130-1 and second chamber 130-2 by two chamber inlets 170 in a parallel configuration. Each chamber is connected to an adjacent chamber by a conduit 172, and in some embodiments, adjacent chambers can be arranged in a parallel configuration by multiple conduits 172.

[0073] Each of the at least three chambers (130-1, 130-2, 130-3) has a surface area, a headspace pressure, and a sublimation rate. As previously described, the sublimation rate of each of the chambers (130-1, 130-2, 130-3) is equal. The sublimation rate is equalized by adjusting one or more of: (1) changing the travel restrictions between the chambers 130; (2) adjusting the relative surface areas of the chambers 130; and (3) adjusting the relative temperature gradients of the chambers 130. Arrangement of the chambers in a series or parallel configuration also affects the sublimation rate. Further subdivision of the container 110 into additional chambers 130 also affects the sublimation rate. The ampoule 100 can have any number of chambers 130, as facilitated by the illustrated configuration of the radial and interior walls.

[0074] The methods, systems, and compositions disclosed herein are not limited to the specific embodiments described herein; rather, method steps, system elements, and / or composition elements may be utilized independently and separately from other steps and / or elements described herein.

[0075] Although specific features of various embodiments may be shown in some drawings and not in others, this is for convenience only. Moreover, references to "one embodiment" in the above description are not intended to be interpreted as excluding the existence of additional embodiments that also incorporate the recited features. In accordance with the principles of the present disclosure, any feature of a drawing may be referenced and / or claimed in combination with any feature of any other drawing.

[0076] This specification uses examples to enable any person skilled in the art to practice the disclosure, including the best mode, including making and using any device or system, and practicing any incorporated methods. The patentable scope of the disclosure is defined by the claims, and may include other examples that occur to those skilled in the art. Such other examples are intended to be within the scope of the claims if they have structural elements that do not differ from the literal language of the claims, or if they contain equivalent structural elements that do not differ substantially from the literal language of the claims.

[0077] Further aspects of the invention are provided by the subject matter of the following clauses.

[0078] A sublimation ampoule comprising: a sublimation vessel having an open end and a closed end, a sidewall, and at least two chambers extending between the open end and the closed end, each chamber separated by a vessel wall, each chamber having a surface area and a sublimation rate; and a vessel lid having a top surface and a bottom surface defining a thickness, the bottom surface being removably securable to the open end of the sublimation vessel forming a fluid seal, the vessel lid having a lid inlet disposed on the top surface of the vessel lid and extending through the thickness; and a lid outlet disposed on the top surface of the vessel lid and extending through the thickness. a container lid comprising: a lid outlet; at least one chamber inlet disposed on a bottom surface of the container lid fluidly connected to the lid inlet, each chamber inlet fluidly connected to one of the at least two chambers, each chamber inlet having a cross-sectional area; and a conduit having a conduit inlet and a conduit outlet disposed on the bottom surface, the conduit inlet and the conduit outlet extending partially into the thickness, the conduit fluidly connecting two of the at least two chambers, the conduit having a cross-sectional area.

[0079] The sublimation ampoule of the preceding clause, wherein the sublimation rate of each chamber is determined by the surface area of ​​each chamber, the temperature of each chamber, and the headspace pressure of each chamber, and the sublimation rate of each chamber is within 20% of the other chambers.

[0080] 10. The sublimation ampoule of any preceding clause, wherein the sublimation rate of each chamber is defined by the surface area of ​​each chamber, the temperature of each chamber, and the headspace pressure of each chamber, and the sublimation rates are equal.

[0081] 10. The sublimation ampoule of any preceding clause, further comprising a heater to facilitate heating of a sidewall of the sublimation vessel.

[0082] 10. The sublimation ampoule of any of the preceding clauses, wherein the sublimation rate in each chamber is equal.

[0083] 10. The sublimation ampoule of any preceding clause, wherein a surface area of ​​the first chamber is equal to a surface area of ​​the second chamber.

[0084] 10. The sublimation ampoule of any preceding clause, wherein the headspace pressure of the first chamber is greater than the headspace pressure of the second chamber.

[0085] 10. The sublimation ampoule of any preceding clause, wherein a cross-sectional area of ​​the conduit connecting the first chamber to the second chamber is smaller than a cross-sectional area of ​​the inlet.

[0086] 10. The sublimation ampoule of any preceding clause, further comprising a radial wall concentric with a central longitudinal axis of the sublimation vessel, the radial wall separating the first chamber from the second chamber, the second chamber adjacent to a side wall of the sublimation vessel.

[0087] 10. The sublimation ampoule of claim 1, wherein the second chamber is heated to a temperature higher than the temperature of the first chamber, and the sidewall of the sublimation vessel is heated by a heater.

[0088] 10. The sublimation ampoule of any preceding clause, wherein the surface area of ​​the first chamber is greater than the surface area of ​​the second chamber.

[0089] 10. The sublimation ampoule of any preceding clause, wherein the headspace pressure of the first chamber is equal to the headspace pressure of the second chamber.

[0090] 10. The sublimation ampoule of any preceding clause, further comprising an inner wall extending across a sidewall of the sublimation vessel, the inner wall separating the first chamber from the second chamber, the first chamber and the second chamber having the same temperature.

[0091] 10. The sublimation ampoule of claim 1, further comprising a radial wall concentric with a central longitudinal axis of the sublimation vessel, the radial wall separating the first chamber from the second chamber, the second chamber adjacent to a side wall of the sublimation vessel, the second chamber being heated at a temperature higher than the temperature of the first chamber, and the side wall of the sublimation vessel being heated by a heater.

[0092] 10. The sublimation ampoule of any preceding clause, wherein the headspace pressure of the first chamber is greater than the headspace pressure of the second chamber.

[0093] 10. The sublimation ampoule of any preceding clause, wherein a cross-sectional area of ​​the conduit connecting the first chamber to the second chamber is smaller than a cross-sectional area of ​​the inlet.

[0094] 10. The sublimation ampoule of any preceding clause, further comprising a second conduit connecting the first chamber to the second chamber.

[0095] 10. The sublimation ampoule of any preceding clause, wherein the closed end of the sublimation vessel is removably securable to the sidewall forming a fluid seal.

[0096] 10. The sublimation ampoule of any preceding clause, further comprising an interior wall extending across a sidewall of the sublimation vessel, the interior wall separating the at least two chambers.

[0097] 10. The sublimation ampoule of any preceding clause, further comprising a plurality of interior walls extending from a central longitudinal axis of the sublimation vessel to a sidewall of the sublimation vessel.

[0098] 10. The sublimation ampoule of any preceding clause, further comprising a radial wall concentric with a central longitudinal axis of the sublimation vessel, the radial wall separating the at least two chambers.

[0099] 10. The sublimation ampoule of claim 1, wherein a second chamber adjacent to the side wall of the sublimation vessel is heated to a temperature higher than the temperature of the first chamber adjacent to the second chamber, and the first chamber is separated from the second chamber by a radial wall.

[0100] 10. The sublimation ampoule of any preceding clause, wherein the lid inlet is fluidly connected to a first chamber of the at least two chambers and the lid outlet is fluidly connected to a second chamber of the at least two chambers.

[0101] 10. The sublimation ampoule of any preceding clause, wherein the third chamber is fluidly connected to the first chamber by a second conduit, the third chamber is fluidly connected to the second chamber by a third conduit, and the second chamber is fluidly connected to the lid outlet.

[0102] 10. The sublimation ampoule of any preceding clause, wherein the lid inlet is fluidly connected to a second chamber inlet of at least one chamber inlet defining a parallel connection of chambers.

[0103] 10. The sublimation ampoule of any preceding clause, wherein the conduit includes a conduit inlet and at least two conduit outlets that define a parallel connection of the chambers.

[0104] 10. The sublimation ampoule of any preceding clause, further comprising at least one chamber outlet fluidly connected to the lid outlet, each chamber outlet fluidly connected to one of the at least two chambers.

[0105] 10. The sublimation ampoule of claim 1, wherein the sublimation vessel is subdivided into four chambers by an inner wall extending across the sidewall of the sublimation vessel and radial walls concentric with a central longitudinal axis of the sublimation vessel.

[0106] 10. The sublimation ampoule of claim 1, wherein the first chamber and the second chamber are separated by an interior wall, the first chamber is in fluid communication with the lid inlet, and the first chamber is in fluid communication with the second chamber by at least one conduit.

[0107] 10. The sublimation ampoule of claim 1, wherein the third and fourth chambers are adjacent to the sidewall of the sublimation vessel and separated from the first and second chambers by a radial wall, the third and fourth chambers are separated by an inner wall, and the fourth chamber is in fluid communication with the lid outlet.

[0108] 10. The sublimation ampoule of any preceding clause, wherein the third chamber and the fourth chamber are in fluid communication by at least one conduit.

[0109] 10. The sublimation ampoule of any preceding clause, wherein the third chamber and the first chamber are in fluid communication by at least one conduit.

[0110] 10. The sublimation ampoule of any preceding clause, wherein the fourth chamber and the second chamber are in fluid communication by at least one conduit.

[0111] 10. The sublimation ampoule of any preceding clause, wherein the third chamber and the fourth chamber are heated to a temperature higher than the temperature of the first chamber and the second chamber.

[0112] 10. The sublimation ampoule of claim 1, wherein the cross-sectional area of ​​the conduit is smaller than the cross-sectional area of ​​the lid inlet.

[0113] 10. The sublimation ampoule of any preceding clause, wherein at least two conduits fluidly connect two of the at least two chambers.

[0114] 10. The sublimation ampoule of any preceding clause, wherein the conduit outlet comprises a showerhead.

[0115] 10. The sublimation ampoule of any preceding clause, wherein the conduit outlet includes a fitting.

[0116] 10. The sublimation ampoule of any preceding clause, wherein the at least one chamber inlet includes a showerhead.

[0117] 10. The sublimation ampoule of any preceding clause, wherein at least one chamber inlet includes a fitting.

[0118] 10. The sublimation ampoule of any preceding clause, wherein the chamber adjacent the outer wall of the sublimation vessel is heated to a temperature higher than the temperature of the chamber separated by the radial wall.

[0119] A sublimation ampoule comprising: a sublimation vessel having an open end and a closed end, a sidewall, and a central longitudinal axis, the sublimation vessel comprising: an inner wall extending across the sidewall of the sublimation vessel; a radial wall concentric with the central longitudinal axis; a first chamber and a second chamber separated by the inner wall; and a third chamber and a fourth chamber separated from the first chamber and the second chamber by the radial wall and adjacent the sidewall of the sublimation vessel; and a vessel lid having a top surface and a bottom surface defining a thickness, the bottom surface being removably securable to the open end of the sublimation vessel forming a fluid seal, the vessel lid having a lid inlet located on the top surface of the vessel lid having a fixed inlet flow rate for allowing fluid to flow through the thickness. a container lid comprising: a lid inlet extending through the thickness; at least one chamber inlet disposed on a bottom surface of the container lid fluidly connected to the lid inlet, the chamber inlet in fluid communication with the first chamber and having a cross-sectional area; a lid outlet disposed on the top surface of the container lid having a fixed outlet pressure, the lid outlet extending through the thickness and in fluid communication with the fourth chamber; and a plurality of conduits having conduit inlets and conduit outlets disposed on the bottom surface, the conduit inlets and conduit outlets extending partially into the thickness, the conduits fluidly connecting to the first chamber, the second chamber, the third chamber, and the fourth chamber, each of the plurality of conduits having a cross-sectional area.

[0120] 10. The sublimation ampoule of any preceding clause, wherein the first chamber is in fluid communication with the second chamber by at least one conduit of the plurality of conduits.

[0121] 10. The sublimation ampoule of any preceding clause, wherein the third chamber and the fourth chamber are in fluid communication by at least one conduit of the plurality of conduits.

[0122] 10. The sublimation ampoule of any preceding clause, wherein the third chamber and the first chamber are in fluid communication by at least one conduit of the plurality of conduits.

[0123] 10. The sublimation ampoule of any preceding clause, wherein the fourth chamber and the second chamber are in fluid communication by at least one conduit.

[0124] 10. The sublimation ampoule of any preceding clause, further comprising a heater configured to heat a sidewall of the sublimation vessel.

[0125] 10. The sublimation ampoule of any preceding clause, wherein the third chamber and the fourth chamber are heated to a temperature higher than the temperature of the first chamber and the second chamber.

[0126] 10. The sublimation ampoule of claim 1, wherein the sublimation rate of each chamber is determined by the surface area of ​​each chamber, the temperature of each chamber, and the headspace pressure of each chamber, and the sublimation rate of each chamber is equal.

[0127] 10. The sublimation ampoule of any of the preceding clauses, wherein the sublimation rate in each chamber is equal.

[0128] 10. The sublimation ampoule of any preceding clause, wherein a surface area of ​​the first chamber is equal to a surface area of ​​the second chamber, and a surface area of ​​the third chamber is equal to a surface area of ​​the second chamber.

[0129] 10. The sublimation ampoule of any preceding clause, wherein the surface area of ​​the first chamber and the second chamber is greater than the surface area of ​​the third chamber and the fourth chamber.

[0130] 10. The sublimation ampoule of any preceding clause, wherein the headspace pressure of the first chamber is greater than the headspace pressure of each of the second chamber, the third chamber, and the fourth chamber.

Claims

1. A sublimation ampoule comprising: a sublimation vessel having an open end and a closed end, a sidewall, and at least two chambers extending between the open end and the closed end, each chamber separated by a vessel wall, each chamber having a surface area and a sublimation rate; a vessel lid having a top surface and a bottom surface defining a thickness, the bottom surface being removably securable to the open end of the sublimation vessel forming a fluid seal, the vessel lid comprising: a lid inlet disposed on the top surface of the container lid, the lid inlet extending through the thickness; a lid outlet disposed on the top surface of the container lid, the lid outlet extending through the thickness; at least one chamber inlet disposed on the bottom surface of the container lid fluidly connected to the lid inlet, each chamber inlet fluidly connected to one of the at least two chambers, each chamber inlet having a cross-sectional area; a conduit having a conduit inlet and a conduit outlet disposed at the bottom surface, the conduit inlet and the conduit outlet extending partially into the thickness, the conduit fluidly connecting two of the at least two chambers, the conduit having a cross-sectional area; a container lid comprising: A sublimation ampoule.

2. 2. The sublimation ampoule of claim 1, wherein the sublimation rate of each chamber is defined by the surface area of ​​each chamber, the temperature of each chamber, and the headspace pressure of each chamber, and the sublimation rate of each chamber is within 20% of the other chambers.

3. 2. The sublimation ampoule of claim 1, wherein the sublimation rate of each chamber is defined by the surface area of ​​each chamber, the temperature of each chamber, and the headspace pressure of each chamber, and the sublimation rates are equal.

4. 10. The sublimation ampoule of claim 1, further comprising a heater for facilitating heating of the sidewall of the sublimation vessel.

5. 5. The sublimation ampoule of claim 4, wherein the sublimation rate in each chamber is equal.

6. 6. The sublimation ampoule of claim 5, wherein the surface area of ​​the first chamber is equal to the surface area of ​​the second chamber.

7. 7. The sublimation ampoule of claim 6, wherein a headspace pressure in the first chamber is greater than a headspace pressure in the second chamber.

8. 8. The sublimation ampoule of claim 7, wherein the cross-sectional area of ​​the conduit connecting the first chamber to the second chamber is smaller than the cross-sectional area of ​​the inlet.

9. 7. The sublimation ampoule of claim 6, further comprising a radial wall concentric with a central longitudinal axis of the sublimation vessel, the radial wall separating the first chamber from the second chamber, the second chamber adjacent the side wall of the sublimation vessel.

10. 10. The sublimation ampoule of claim 9, wherein the second chamber is heated to a temperature higher than the temperature of the first chamber, and the sidewall of the sublimation vessel is heated by a heater.

11. 6. The sublimation ampoule of claim 5, wherein the surface area of ​​the first chamber is greater than the surface area of ​​the second chamber.

12. 12. The sublimation ampoule of claim 11, wherein the headspace pressure of the first chamber is equal to the headspace pressure of the second chamber.

13. 12. The sublimation ampoule of claim 11, further comprising an interior wall extending across the sidewall of the sublimation vessel, the interior wall separating the first chamber from the second chamber, the first chamber and the second chamber having the same temperature.

14. 12. The sublimation ampoule of claim 11, further comprising a radial wall concentric with a central longitudinal axis of the sublimation vessel, the radial wall separating the first chamber from the second chamber, the second chamber adjacent to the side wall of the sublimation vessel, the second chamber being heated at a temperature higher than the temperature of the first chamber, and the side wall of the sublimation vessel being heated by a heater.

15. 15. The sublimation ampoule of claim 14, wherein the headspace pressure in the first chamber is greater than the headspace pressure in the second chamber.

16. 16. The sublimation ampoule of claim 15, wherein the cross-sectional area of ​​the conduit connecting the first chamber to the second chamber is smaller than the cross-sectional area of ​​the inlet.

17. 16. The sublimation ampoule of claim 15, further comprising a second conduit connecting the first chamber to the second chamber.

18. 10. The sublimation ampoule of claim 1, wherein the closed end of the sublimation vessel is removably securable to the sidewall forming a fluid seal.

19. 10. The sublimation ampoule of claim 1, further comprising an interior wall extending across the sidewall of the sublimation vessel, the interior wall separating the at least two chambers.

20. 10. The sublimation ampoule of claim 1, further comprising a plurality of interior walls extending from a central longitudinal axis of the sublimation vessel to the side walls of the sublimation vessel.

21. 10. The sublimation ampoule of claim 1, further comprising a radial wall concentric with a central longitudinal axis of said sublimation vessel, said radial wall separating said at least two chambers.

22. 22. The sublimation ampoule of claim 21, wherein a second chamber adjacent the side wall of the sublimation vessel is heated to a temperature higher than the temperature of a first chamber adjacent the second chamber, and the first chamber is separated from the second chamber by the radial wall.

23. 10. The sublimation ampoule of claim 1, wherein the lid inlet is fluidly connected to a first chamber of the at least two chambers and the lid outlet is fluidly connected to a second chamber of the at least two chambers.

24. 24. The sublimation ampoule of claim 23, wherein a third chamber is fluidly connected to the first chamber by a second conduit, the third chamber is fluidly connected to the second chamber by a third conduit, and the second chamber is fluidly connected to the lid outlet.

25. 3. The sublimation ampoule of claim 2, wherein the lid inlet is fluidly connected to a second chamber inlet of the at least one chamber inlet defining a parallel connection of chambers.

26. 10. The sublimation ampoule of claim 1, wherein the conduit includes a conduit inlet and at least two conduit outlets that define a parallel connection of chambers.

27. 10. The sublimation ampoule of claim 1, further comprising at least one chamber outlet fluidly connected to the lid outlet, each chamber outlet fluidly connected to one of the at least two chambers.

28. 10. The sublimation ampoule of claim 1, wherein the sublimation vessel is subdivided into four chambers by interior walls extending across the side walls of the sublimation vessel and radial walls concentric with a central longitudinal axis of the sublimation vessel.

29. 30. The sublimation ampoule of claim 28, wherein a first chamber and a second chamber are separated by the interior wall, the first chamber is in fluid communication with the lid inlet, and the first chamber is in fluid communication with the second chamber by at least one conduit.

30. 30. The sublimation ampoule of claim 29, wherein a third chamber and a fourth chamber are adjacent to the side wall of the sublimation vessel and separated from the first chamber and the second chamber by the radial wall, the third chamber and the fourth chamber are separated by the interior wall, and the fourth chamber is in fluid communication with the lid outlet.

31. 31. The sublimation ampoule of claim 30, wherein the third chamber and the fourth chamber are in fluid communication by at least one conduit.

32. 31. The sublimation ampoule of claim 30, wherein the third chamber and the first chamber are in fluid communication by at least one conduit.

33. 31. The sublimation ampoule of claim 30, wherein the fourth chamber and the second chamber are in fluid communication by at least one conduit.

34. 31. The sublimation ampoule of claim 30, wherein the third and fourth chambers are heated to a temperature greater than the temperature of the first and second chambers.

35. 2. The sublimation ampoule of claim 1, wherein the cross-sectional area of ​​the conduit is smaller than the cross-sectional area of ​​the lid inlet.

36. 10. The sublimation ampoule of claim 1, wherein at least two conduits fluidly connect two of the at least two chambers.

37. 10. The sublimation ampoule of claim 1, wherein the conduit outlet comprises a showerhead.

38. The sublimation ampoule of claim 1 , wherein the conduit outlet includes a fitting.

39. The sublimation ampoule of claim 1 , wherein the at least one chamber inlet comprises a showerhead.

40. The sublimation ampoule of claim 1 , wherein the at least one chamber inlet includes a fitting.

41. 41. The sublimation ampoule of claim 40, wherein a chamber adjacent to the outer wall of the sublimation vessel is heated to a temperature greater than the temperature of the chamber separated by the radial wall.

42. A sublimation ampoule comprising: A sublimation vessel having an open end and a closed end, a sidewall, and a central longitudinal axis, an inner wall extending across the side wall of the sublimation vessel; a radial wall concentric with the central longitudinal axis; a first chamber and a second chamber separated by the inner wall; a third chamber and a fourth chamber separated from the first chamber and the second chamber by the radial walls and adjacent to the side wall of the sublimation vessel; a sublimation vessel comprising: a vessel lid having a top surface and a bottom surface defining a thickness, the bottom surface being removably securable to the open end of the sublimation vessel forming a fluid seal, the vessel lid comprising: a lid inlet disposed on the top surface of the container lid having a fixed inlet flow rate, the lid inlet extending through the thickness; at least one chamber inlet disposed on the bottom surface of the container lid fluidly connected to the lid inlet, the chamber inlet being in fluid communication with the first chamber and having a cross-sectional area; a lid outlet disposed on the top surface of the container lid having a fixed outlet pressure, the lid outlet extending through the thickness and in fluid communication with the fourth chamber; a plurality of conduits having conduit inlets and conduit outlets disposed in the bottom surface, the conduit inlets and conduit outlets extending partially into the thickness, the conduits fluidly connecting the first chamber, the second chamber, the third chamber, and the fourth chamber, each of the plurality of conduits having a cross-sectional area; a container lid comprising: A sublimation ampoule.

43. 43. The sublimation ampoule of claim 42, wherein the first chamber is in fluid communication with the second chamber by at least one conduit of the plurality of conduits.

44. 43. The sublimation ampoule of claim 42, wherein the third chamber and the fourth chamber are in fluid communication by at least one conduit of the plurality of conduits.

45. 43. The sublimation ampoule of claim 42, wherein the third chamber and the first chamber are in fluid communication by at least one conduit of the plurality of conduits.

46. 43. The sublimation ampoule of claim 42, wherein the fourth chamber and the second chamber are in fluid communication by at least one conduit.

47. 43. The sublimation ampoule of claim 42, further comprising a heater configured to heat the sidewall of the sublimation vessel.

48. 48. The sublimation ampoule of claim 47, wherein the third chamber and the fourth chamber are heated to a temperature greater than the temperature of the first chamber and the second chamber.

49. 49. The sublimation ampoule of claim 48, wherein the sublimation rate of each chamber is defined by the surface area of ​​each chamber, the temperature of each chamber, and the headspace pressure of each chamber, and wherein the sublimation rate of each chamber is equal.

50. 50. The sublimation ampoule of claim 49, wherein the sublimation rate in each chamber is equal.

51. 50. The sublimation ampoule of claim 49, wherein the surface area of ​​the first chamber is equal to the surface area of ​​the second chamber, and the surface area of ​​the third chamber is equal to the surface area of ​​the second chamber.

52. 50. The sublimation ampoule of claim 49, wherein the surface area of ​​the first chamber and the second chamber is greater than the surface area of ​​the third chamber and the fourth chamber.

53. 50. The sublimation ampoule of claim 49, wherein the headspace pressure in the first chamber is greater than the headspace pressure in each of the second chamber, the third chamber, and the fourth chamber.

Images