TW201330057A - Apparatus for sublimating solid state precursors - Google Patents

Abstract

In some embodiments, an apparatus for sublimating solid state precursors may include a container having a body, lid, and removable bottom, wherein the removable bottom is sealable to the body to seal the container when coupled to the body; a tray insertable into the container from a bottom of the container, the tray comprising: a gas permeable base to support a solid state precursor, the gas permeable base having a through hole disposed proximate the center of the gas permeable base; an outer ring disposed around an outer edge of the base and extending upwardly from the base, the outer ring configured to interface with the lid of the container; and an inner ring disposed within the through hole, the inner ring configured to interface with the lid of the container; an inlet disposed through the lid of the container; and an outlet disposed through the lid of the container.

Description

Equipment for sublimating solid state precursors

Embodiments of the invention relate generally to semiconductor processing.

The inventors of the present invention have observed precursor systems that have been conventionally used for deposition processes (eg, epitaxial growth or atomic layer deposition processes) (eg, gases, liquid vapors, liquid/inert gas carriers, solids evaporation, solids). Sublimation, reactive carriers, etc.) provide precursors that are not sufficiently pure for current semiconductor processing requirements. Again, previously prepared precursors that are conventionally used are unstable and will decompose, coagulate or change state over time.

Therefore, the inventors of the present invention have provided improved apparatus for transporting precursors which have improved purity compared to conventionally produced precursors.

Equipment for sublimating solid precursors is provided herein. In some embodiments, an apparatus for sublimating a solid precursor can include: a container having a body, a cover, and a removable bottom, wherein the removable bottom Sealable to the body to seal the container when the removable bottom is coupled to the body; a tray insertable from a bottom of the container into the container, wherein the tray can include: a gas Permeating a substrate, the gas permeable substrate for supporting a solid precursor, the gas permeable substrate having a perforation disposed adjacent the center of the gas permeable substrate; and an outer ring surrounding the substrate An outer edge is disposed and extends upwardly from the base, the outer ring is configured to form an interface with the cover of the container; and an inner ring is disposed in the through hole, the inner ring being disposed with the container The lid forms an interface one-to-one inlet, the inlet being disposed through the lid of the container, the inlet being provided to provide a gas to an area under the tray via the inner ring of the tray; and an outlet configured to pass the outlet The lid of the container is capable of allowing the solid precursor in the form of a gas to flow out of the container.

In some embodiments, an apparatus for sublimating a solid precursor can include: a container having a body, a cover and a removable bottom, the removable bottom being sealable to the body to be The container is sealed when the bottom portion is coupled to the body; a first tray is insertable into the container from a bottom of the container, the first tray comprising a gas permeable substrate and an inner wall And an outer wall, wherein the gas permeable substrate is for supporting a solid precursor and has a central opening formed through the substrate, the inner wall being disposed around the central opening of the substrate, the outer wall surrounding the substrate An outer edge, wherein the inner wall forms an interface with the outer wall and the lid of the container to provide a hermetic seal between the first tray and the lid; an inlet disposed through the lid of the container And coupled to an input channel to provide a gas to an area below the first disk, wherein the input channel passes through the central opening of the substrate And at least partially defined by the inner wall of the first disk; and an outlet disposed through the cover of the container and located generally between the inner wall of the first disk and the outer wall In a region above an area of the first disk, the solid precursor in the form of a permissible gas can flow out of the container.

Other and further embodiments of the invention are described below.

100‧‧‧Processing chamber

101‧‧‧Substrate

102‧‧‧ upper

104‧‧‧ lower

106‧‧‧ Cover

108‧‧‧ clamping ring

110‧‧‧ chamber body

112‧‧‧floor

114‧‧‧Inhalation test

116‧‧‧ lining

117‧‧‧ gas source

118‧‧‧Emissions埠

119‧‧‧vacuum pump

120‧‧‧ enclosure

121‧‧‧Bottom plate assembly

122‧‧‧Preheating ring

123‧‧‧vacuum system

124‧‧‧Substrate support

126‧‧‧Substrate lifting rod

127‧‧‧shims

128‧‧‧ upper

130‧‧‧Support system

132‧‧‧ Lower Dome

134‧‧‧Support bracket

136‧‧‧Upheating lamp

138‧‧‧Upheating lamp

140‧‧‧ Controller

142‧‧‧Central Processing Unit (CPU)

144‧‧‧ memory

146‧‧‧Support circuit

152‧‧‧Under heat lamp

154‧‧‧Under heat lamp

156‧‧‧Upper pyrometer

158‧‧‧ under the pyrometer

160‧‧‧Substrate lifting assembly

161‧‧‧ Lifting pin module

162‧‧‧ first opening

164‧‧‧Substrate support assembly

166‧‧‧Support pin

180‧‧‧ Equipment

202‧‧‧ shell

204‧‧‧ lining

206‧‧‧ Subject

208‧‧‧

210‧‧‧ Container

212‧‧‧ gas tube

213‧‧‧Area

215‧‧‧ bottom plate

216‧‧‧ bottom

218‧‧‧ Seals

219‧‧‧ outer edge

220, 221, 223, 225, 227‧ ‧ pressure monitors

222‧‧‧outer ring (outer wall)

224‧‧‧ Temperature Control Unit

226‧‧‧ Cover

228‧‧‧ bottom

230‧‧‧ entrance

231‧‧‧ bottom

232‧‧‧Export

234‧‧‧ outer surface

236‧‧‧ top

240‧‧‧ Inner ring (or inner wall)

241‧‧‧Circle Room

242‧‧‧ Gas permeable substrate

243‧‧‧Perforation

245‧‧‧Overlay block

246‧‧‧ Temperature Control Mechanism

247‧‧‧ pressure gauge

248‧‧‧ Temperature Control Mechanism

249‧‧‧ pressure gauge

302‧‧‧base part

304‧‧‧Outward extension

306‧‧‧ base part

308‧‧‧Outward extension

310‧‧‧ recess

312‧‧ ‧ pocket

Embodiments of the invention may be understood by reference to the exemplary embodiments of the invention, which are briefly described above and discussed in more detail below, wherein the exemplary embodiments are illustrated in the drawings Illustration. It is to be understood, however, that the appended claims

Figure 1 illustrates a process chamber suitable for use with equipment for sublimating solid state precursors in accordance with some embodiments of the present invention.

Figure 2 illustrates an apparatus for sublimating a solid state precursor in accordance with some embodiments of the present invention.

Figure 3 illustrates a disk for use in an apparatus for sublimating solid state precursors in accordance with some embodiments of the present invention.

To promote understanding, the same element symbols are used where possible to indicate the same elements that are common to the drawings. The drawings are not drawn to scale and may be simplified for clarity. It is contemplated that elements and features of one embodiment may be beneficially incorporated into other embodiments without particular detail.

Equipment for sublimating solid precursors is provided herein. In some embodiments, the apparatus of the present invention may advantageously provide one or more solid precursor support trays that are easily attached to and removed from the apparatus, thereby providing easier and more conventional switching sublimation systems than conventional apparatus. An efficient mechanism for providing solid precursors to solid state precursor sublimation systems. The apparatus of the present invention may more advantageously provide a point of use for precursor generation, thereby reducing the risk of precursor condensation, changing state, or dispersing system reactions. The apparatus of the present invention may more advantageously provide a pressure gradient within the apparatus to promote sublimation of a more uniform solid precursor, thereby providing improved process consistency and material applicability. While not wishing to be bound by a scope, the inventors have observed that the apparatus of the present invention can be used to provide precursors for epitaxial and atomic layer deposition processes.

1 illustrates a schematic side view of a process chamber 100 suitable for use with equipment for sublimating solid state precursors, in accordance with some embodiments of the present invention. In some embodiments, the process chamber 100 can be a commercially available process chamber, such as an EPI® reactor available from Applied Materials, Inc. of Santa Clara, Calif., or has been modified and described herein. The precursor transport apparatus is used in conjunction with any suitable semiconductor processing chamber suitable for performing an epitaxial germanium deposition process. However, other process chambers can also be used.

The process chamber 100 can generally include a chamber body 110, a support system 130, and a controller 140. Apparatus 180 for sublimating the solid state precursor may be coupled to process chamber 100 via, for example, a process gas suction port or inlet 114. Apparatus 180 for sublimating solid state precursors can generally be used to sublimate any compatible type of solid precursor required for use in a desired application, such as the exemplary embodiments described below. Solid precursor.

The chamber body 110 generally includes an upper portion 102, a lower portion 104, and a surrounding body 120. Vacuum system 123 can be coupled to chamber body 110 to promote maintenance of the desired pressure within chamber body 110. In some embodiments, the vacuum system 123 can include a throttle valve (not shown) and a vacuum pump 119 for pumping the chamber body 110. In some embodiments, the pressure within the chamber body 110 can be adjusted by adjusting the throttle and/or vacuum pump 119. Upper portion 102 is disposed on lower portion 104, and upper portion 102 includes cover 106, clamping ring 108, inner liner 116, bottom plate 112, one or more upper heat lamps 136, and one or more lower heat lamps 152 and upper pyrometer 156. In some embodiments, the cover 106 has a dome-like form factor, however a cover having other form factors (eg, a flat or inverted cover) is also contemplated. The lower portion 104 is coupled to the process gas suction port 114 and the discharge port 118, and the lower portion 104 includes a bottom plate assembly 121, a lower dome 132, a substrate support 124, a preheat ring 122, a substrate lifting assembly, a substrate support assembly 164, One or more upper heater lamps 138 and one or more lower heater lamps 154 and lower pyrometer 158. Although the term "ring" is used to describe a particular component of process chamber 100, such as preheat ring 122, it is contemplated that the shape of the members need not be circular and may include any shape (including but not limited to rectangular , polygons, ellipses, and the like).

The substrate 101 is disposed on the substrate support 124 during processing. Lamps 136, 138, 152, and 154 are sources of infrared (IR) radiation (e.g., heat) and produce a predetermined temperature distribution throughout substrate 101 during operation. The cover 106, the clamping ring 108 and the lower dome 132 are formed of quartz, although other infrared transmissive and process compatible materials may be used to form the members.

The substrate support assembly 164 generally includes a support bracket 134 having a plurality of support pins 166 coupled to the substrate support 124. The substrate lifting assembly 160 includes a substrate lifting bar 126 and a plurality of lifting pin modules 161 that are selectively disposed on respective pads 127 of the substrate lifting bar 126. In one embodiment, the lift pin module 161 includes an optional upper portion of the lift pin 128 that is movably disposed past the first opening 162 in the substrate support 124. In operation, the substrate lifter 126 is moved to engage the lift pins 128. When engaged, the lift pins 128 can raise the substrate 101 above the substrate support 124 or lower the substrate 101 onto the substrate support 124.

Support system 130 includes components for performing and monitoring a predetermined process (eg, growing an epitaxial film) in process chamber 100. Such components generally include various subsystems (eg, gas panels, gas distribution conduits, vacuum and exhaust subsystems, and the like) and devices of the process chamber 100 (eg, power supplies, process control facilities, and the like). Such components are well known to those skilled in the art and are omitted from the drawings for clarity.

A controller 140 can be provided and coupled to the process chamber 100 to control components of the process chamber 100. Controller 140 can be any suitable controller for controlling the operation of the substrate processing chamber. The controller 140 generally includes a central processing unit (CPU) 142, a memory 144 and a support circuit 146, and the controller 140 is directly coupled to and controls the process chamber 100 and the support system 130 (as shown in FIG. 1). Alternatively, the process chamber 100 and the support system 130 are coupled to and controlled via a computer (or controller) associated with the process chamber and/or support system.

The CPU 142 can be any form of general purpose computer processor used in industrial equipment. Support circuitry 146 is coupled to CPU 142 and may include cache, clock circuitry, input/output subsystems, power supplies, and the like. A software routine (such as the method disclosed herein below for processing a substrate as disclosed in FIG. 2) may be stored in the memory 144 of the controller 140. When the software routine is executed by the CPU 142, the software routine converts the CPU 142 into a special purpose computer (controller) 140. The software routine can also be stored and/or executed by a second controller (not shown) located remotely from the controller 140. Alternatively or in combination, in some embodiments (eg, process chamber 100 is part of a multi-chamber processing system), each process chamber of the multi-chamber processing system may have its own controller for controlling the text herein Portions of the inventive method that can be performed in this particular processing chamber are disclosed. In such embodiments, individual controllers can be arranged in a manner similar to controller 140 and can be coupled to controller 140 to synchronize the operation of process chamber 100.

A gas source 117 can be coupled to the apparatus 180 for sublimating the solid precursor to provide one or more gases to facilitate sublimation of the solid precursor and/or delivery of the sublimated precursor (as described below). For example, in some embodiments, gas source 117 can provide a reactive gas such as hydrogen (H ₂ ), hydrogen chloride (HCl), chlorine (Cl ₂ ), bromine (Br), oxygen (O ₂ ), methane (CH _{4 )} ) or the like. Alternatively or in combination, in some embodiments, the gas source may provide an inert gas or carrier gas, such as helium (He), argon (Ar), xenon (Xe), or the like.

Referring to FIG. 2, apparatus 180 for sublimating solid state precursors can generally include a container 210, one or more trays 208 (four trays are shown), an inlet 230 and an outlet 232.

The container 210 generally includes a body 206, a lid 226 and a removable bottom 228 that is configured to seal the container 210 when the bottom 228 is coupled to the body 206. In some embodiments, the cover 226 can include an inlet 230 for providing gas to the container 210 and an outlet 232 for allowing a solid precursor in gaseous form to flow out of the container 210. In some embodiments, each of inlet 230 and outlet 232 can include or can be coupled to temperature control mechanisms 246, 248 (eg, heaters) to control the temperature of the gas flowing through each of inlet 230 and outlet 232. . In some embodiments, a pressure gauge (eg, 247, 249) can be coupled to each of inlet 230 and outlet 232 to allow pressure within vessel 210 to be monitored. By monitoring the pressure within the container 210, the amount of precursor within the container 210 can also be monitored. Container 210 may be made of any material that does not react with the precursor to be sublimed (e.g., the precursors discussed below). For example, in some embodiments, the container 210 can be made of quartz or stainless steel.

The one or more discs 208 can be inserted into the container 210 from the bottom 231 of the container 210. By arranging the one or more discs in this manner, the inventors have observed that the one or more discs 208 can be easily and quickly provided to the device 180 for sublimating the solid precursor. The device 180 is removed, thereby providing a mechanism for providing solid precursors to the solid precursor sublimation system 180 that is easier and more efficient than conventional precursor sublimation systems.

Although four disks 208 are shown in the figures, any number of disks 208 needed to perform the desired sublimation process can be provided. For example, in some embodiments, fewer than four (such as one, two, or three) disks 208 may be provided. Alternatively, in some embodiments, more than four disks 208 may be provided.

Each disk 208 generally includes a gas permeable with perforations 243 The substrate 242, an outer ring 222 (or outer wall) disposed around the outer edge 219 of the gas permeable substrate 242, and an inner ring 240 (or inner wall) disposed within the perforations 243. Outer ring 222 and inner ring 240 may be made of any material that does not react with the particular precursor used to sublimate (e.g., the precursors discussed below). For example, in some embodiments, outer ring 222 and inner ring 240 can be made of quartz or stainless steel. In some embodiments, outer ring 222 and inner ring 240 may interface with cover 226 of container 210 to provide a hermetic seal between disk 208 and cover 226, while promoting gas (eg, sublimated precursor) toward the outlet The flow of 232. Alternatively or in combination, in some embodiments (eg, device 180 for sublimating solid state precursors includes a plurality of disks 208 stacked on one another in container 210 (eg, as shown in FIG. 2), outer ring Each of the 222 and inner ring 240 can form an interface with the outer ring 222 of the other disk disposed directly on the disk 208 and the inner ring 240. For example, in some embodiments (such as shown in FIG. 3), outer ring 222 and inner ring 240 can each comprise a base portion (eg, base portion 302, 306) having a protrusion from a respective base portion Outwardly extending sheets 304, 308. The outwardly extending sheets 304, 308 can be configured to form an interface with respective pockets (e.g., pockets 310, 312) formed in the bottom portion of the base portion of the other tray, the other tray being configured to serve the trays The hermetic sealing between the disks 208 is facilitated when 208 are stacked on one another.

The inventors of the present invention have observed that conventional precursor ampoules heated by external heat sources typically exhibit slow temperature response times due to poor thermal coupling. Thus, and referring back to FIG. 2, in some embodiments, temperature control unit 224 can be disposed within annular chamber 241 formed by inner ring 240 to facilitate control of various trays within container 210 and/or disposed within container 210. Temperature within 208 degree. By controlling the temperature from within the container (i.e., within the ring chamber 241, as shown), the inventors have observed that the temperature response time can be improved compared to conventional methods of heating precursor ampoules. This provides improved temperature control compared to their conventional methods.

Temperature control unit 224 can include any mechanism suitable for controlling the temperature within container 210. For example, in some embodiments, temperature control unit 224 can include an active temperature control system, such as a heater (such as a resistive heater). Alternatively or in combination, in some embodiments, temperature control unit 224 can include a passive temperature control system, such as a series of conduits that are configured to allow temperature control fluid to flow through temperature control unit 224.

Gas source 117 provides the one or more gases (eg, one or more gases discussed above) to ring chamber 241 via inlet 230 and to the bottommost disk of the one or more disks 208 (eg, The area 213 below the disk 215). For example, in some embodiments, the input channel can pass through a central opening of the base of the disk. The input channel can be at least partially defined by an inner wall or inner ring of the disk 208 to provide the one or more gases to the area below the disk. In some embodiments, a gas manifold 212 can be disposed within region 213 below the bottommost disk 215 and coupled to the annulus to provide a uniform gas distribution to the one or more disks 208. The gas manifold 212 can be made of any material that does not react with the gas provided by the gas source, such as quartz or stainless steel.

The gas permeable substrate 242 supports the solid precursor and allows the sublimated solid precursor to pass. The gas permeable substrate 242 can comprise any material suitable for allowing a gas (eg, a sublimated precursor) to flow through the gas permeable substrate 242. For example, in some embodiments, the gas permeable substrate 242 can comprise a block Frit, such as quartz block or stainless steel block. In such embodiments, the block may comprise any pore size suitable for allowing the sublimated precursor stream to pass through the block while substantially avoiding the larger particle solid precursor stream passing through the gas permeable substrate 242. For example, in some embodiments, the block may comprise a pore size of from about 25 to about 150 microns or, in some embodiments, about 100 microns.

In some embodiments, by varying the pore size of the gas permeable substrate 242 of each disk 208, the pressure within each disk 208 can be controlled, thereby allowing the rate of sublimation of the solid precursor within each disk 208 to be controlled. For example, as the pore size of the gas permeable substrate 242 of the disk 208 decreases, the pressure within the disk increases and the rate of reaction of the precursor within the disk decreases.

The inventors of the present invention have observed that in a conventional precursor sublimation system using multiple platforms (e.g., shelves), the solid precursor in the first platform is consumed from the first platform at a higher rate than the later platform. Due to the difference in the rate of consumption of this solid precursor with the change in solid precursor filler over time, the solid precursor in the later stage needs to be impacted in order to place the material and restore the sublimation rate, thus rendering the process inefficient. Accordingly, the inventors of the present invention have observed that by establishing a pressure gradient across the disk 208 (e.g., by varying the pore size of the gas permeable substrate 242 of each disk 208), wherein the lowermost disk of the disk 208 With the highest pressure and the lowest disc of the disc 208 having the lowest pressure, the rate of consumption of the solid precursor in each disc 208 can be more uniform, thereby providing a more consistent sublimation rate across all of the discs and allowing The maximum solid precursor utilization rate before refilling and replacing the disk 208 improves the process consistency of the sublimation process and increases the efficiency of the sublimation process.

In some embodiments, the overlay block (at the symbol 245 in the figure) The dashed line illustration can be disposed on the gas permeable substrate 242. The cover block 245 can be made of the same material as the gas permeable substrate 242 discussed above, or in some embodiments can be made of a different material than the gas permeable substrate 242 discussed above. In addition, the cover block 245 can include any pore size suitable for permitting sublimation of the precursor stream through the cover block 245 (eg, within the pore size range discussed above with respect to the gas permeable substrate 242). When present, a solid precursor can be disposed between the gas permeable substrate 242 and the cover block 245, thereby allowing the disk 208 to be "prefilled" or loaded with a precursor prior to use. In some embodiments, the pre-filled disk can be hermetically sealed to reduce exposure of the precursor to the atmosphere outside of the container 210, thereby increasing the stability of the precursor and reducing decomposition of the precursor. In such embodiments, the hermetic seal (e.g., the detachable disc) may be destroyed prior to use of the disc.

In some embodiments, a pressure monitor (pressure monitor 220, 221, 223, 225, 227) can be coupled to each of the one or more disks 208 to monitor inter-platform pressure (at the one or more The pressure within each of the plurality of disks 208). The amount of precursor disposed on each of the one or more disks 208 can be monitored by monitoring the pressure at each of the one or more disks 208.

In some embodiments, the shell 202 can be disposed around the outer surface 234 of the container 210. The housing 202 generally includes a body 206, a bottom 216, and an optional top (illustrated in phantom at symbol 236 in the figure). In some embodiments, the seal 218 can be disposed between the bottom 216 and the body 206 and/or between the top 236 and the body 206 to provide a vacuum seal between the components of the shell 202. Seal 218 can be any type of seal, such as an O-ring made of, for example, a high temperature resistant polymer such as polytetrafluoroethylene (PTFE).

When present, the shell 202 can promote elevated control of the temperature of the container by increasing or decreasing the rate of heat transfer to or from the container 210 during use. For example, in some embodiments, the shell 202 can comprise an insulating material to reduce heat loss from the container 210, thus allowing the container 210 to be maintained at a higher temperature without the need for additional heating. Alternatively or in combination, the shell 202 can provide active heating or cooling of the container 210. For example, in some embodiments, the shell 202 can include one or more conduits disposed within the housing and configured to allow heat transfer fluid to flow through the shell 202. Alternatively or in combination, in some embodiments, the shell 202 can include one or more inline heaters (such as resistive heaters or the like). In some embodiments, an external heat source, such as an IR lamp, can be disposed outside of the shell 202 to provide thermal energy to the shell 202. In some embodiments, the liner 204 can be disposed between the shell 202 and the container 210. The liner 204 can be made of any material (e.g., quartz) suitable for providing a desired amount of heat transfer.

Upon preparation of the apparatus 180 for sublimating the solid precursor, the one or more discs 208 are first loaded with a solid precursor (such as a powdered, pelletized or sintered solid precursor). The disks 208 are then stacked on the bottom plate 228 and snapped together (e.g., via matching the features of the sheets 304, 308 and the pockets 310, 312 as described above). The tray 208 and bottom plate 228 can then be mounted into the body 206 of the container 210. The vessel 210 can then optionally be purged and pressurized with an inert gas such as helium (He), argon (Ar), xenon (Xe), or the like. When pressurized, an odorizing program can be utilized to determine if the container 210 is airtight. The pressure drop within the vessel is then recorded in vessel 310 to provide a baseline pressure followed by a determination of the consumption of solid precursor. Apparatus 180 for sublimating the solid state precursor is then installed into the processing system (eg, coupled to the process chamber as described above) 100). Process parameters (eg, process gases, pressures and temperatures required for sublimation, or the like) are then determined and entered into a controller (eg, controller 140 as described above). The initial process conditions of the sublimation process can begin.

At operation of the apparatus 180 for sublimating the solid precursor, one or more process gases provided by the gas source 117 are provided to the annulus 241 formed by the inner ring 240 of the one or more discs 208. The one or more process gases flow down the ring chamber 241 to a region 213 below the bottommost disk (eg, disk 215) of the one or more disks 208 and are spread to the bottommost disk. Gas manifold 212 provides a uniform distribution of the one or more gases to the bottom tray. The one or more process gases then pass through the gas permeable substrate 242 and pass up through the one or more disks 208 in the vessel to react with the sublimated precursor or carry the sublimated precursor (where the sublimation can be borrowed Controlled by one or more reactions, temperatures or pressures at the various disks 208 and the one or more process gases). The sublimated precursor then flows to the outlet 232 and is provided to the process chamber 100.

In an exemplary application of apparatus 180 for sublimating solid state precursors as described above, in some embodiments, apparatus 180 for sublimating solid state precursors can be used to provide tin (Sn) precursors to the process chamber. The inventors of the present invention have observed that tin (Sn) can be used as a stressor in a particular deposition process, such as in a germanium (Ge) epitaxial or atomic layer deposition (ALD) process. However, ultra-high purity precursors are not readily available. Further, the previously prepared tin hydride (for example, stannous (SnH ₄ )) is unstable, and the organotin compound contains a large amount of carbon which is not allowed. Thus, in some embodiments, apparatus 180 for sublimating solid state precursors can be used as a point of use precursor source to provide tin (Sn) precursors, including high purity precursors. For example, in such embodiments, a solid tin (Sn) precursor can be provided to disk 208 and include one of hydrogen chloride gas (HCl), chlorine (Cl ₂ ), heavy hydrogen (D), or hydrogen (H ₂ ). Process gases of more or more may be provided to the vessel 210. Next, a tin precursor can be generated according to the following equation: (1) Sn(s) + 2HCl(G) → SnCl ₂ + H ₂ (G)

(2) Sn(s)+2Cl ₂ (G) → SnCl ₄ (G)

(3) Sn(s)+2H ₂ (G) → SnH ₄ (G)

(4) Sn(s)+2D(G) → SnD ₄ (G)

In another exemplary application of apparatus 180 for sublimating solid state precursors as described above, in some embodiments, apparatus 180 for sublimating solid state precursors can be utilized to provide a series of steps for multi-step reactions. Conversion. In such embodiments, the various disks 208 of the device 180 for sublimating the solid precursor may be used to perform one step of the multi-step reaction, or in some embodiments, a single device 180 for sublimating the solid precursor may be used to perform A step in a multi-step reaction. An exemplary multi-step reaction can include a first step of producing a precursor, a second step of converting the precursor, and a third step of purifying the precursor. For example, in some embodiments, the device 180 for sublimation of solid precursor used to lithium aluminum hydrate (LiAlH ₄₎ to produce a tin precursor (e.g., SnH _4).

In such embodiments, the solid tin (Sn) precursor may be provided to the one or more first disk plate 208, lithium aluminum hydrate (LiAlH ₄₎ may be provided to the one or more disks The second disk of 208, and the third disk can serve as a cold disk to capture undesirable solids. Next, a tin precursor can be produced according to the following equation/step: (1) Sn(s)+2Cl ₂ (g) → SnCl ₄ (G)

_{(2) SnCl 4 (G)} + LiAlH 4 (s) → SnH 4 (G) + LiCl (S) + AlCl 3 (s)

(3) Solid AlCl ₃ (s) is captured in the topmost plate

Accordingly, apparatus for sublimating solid state precursors has been provided herein. In some embodiments, the apparatus of the present invention may advantageously provide one or more solid precursor support trays that are easily attached to and removed from the apparatus, thereby providing easier and more conventional switching sublimation systems than conventional apparatus. An efficient mechanism for providing solid precursors to solid state precursor sublimation systems. The apparatus of the present invention may more advantageously provide a point of use for precursor generation, thereby reducing the risk of precursor condensation, changing state, or dispersing system reactions. The apparatus of the present invention may more advantageously provide a pressure gradient within the apparatus to promote sublimation of a more uniform solid precursor, thereby providing improved process consistency and material applicability.

While the above description is directed to embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the scope of the invention.

100‧‧‧Processing chamber

117‧‧‧ gas source

180‧‧‧ Equipment

202‧‧‧ shell

204‧‧‧ lining

206‧‧‧ Subject

208‧‧‧

210‧‧‧ Container

212‧‧‧ gas tube

213‧‧‧Area

215‧‧‧ bottom plate

216‧‧‧ bottom

218‧‧‧ Seals

219‧‧‧ outer edge

220, 221, 223, 225, 227‧ ‧ pressure monitors

222‧‧‧outer ring (outer wall)

224‧‧‧ Temperature Control Unit

226‧‧‧ Cover

228‧‧‧ bottom

230‧‧‧ entrance

231‧‧‧ bottom

232‧‧‧Export

234‧‧‧ outer surface

236‧‧‧ top

240‧‧‧ Inner ring (or inner wall)

241‧‧‧Circle Room

242‧‧‧ Gas permeable substrate

243‧‧‧Perforation

245‧‧‧Overlay block

246‧‧‧ Temperature Control Mechanism

247‧‧‧ pressure gauge

248‧‧‧ Temperature Control Mechanism

249‧‧‧ pressure gauge

Claims (20)

An apparatus for sublimating a solid state precursor, comprising: a container having a body, a cover and a removable bottom, wherein the removable bottom is sealable to the body to be coupled at the removable bottom The container can be sealed to the body; a tray can be inserted into the container from a bottom of the container, the tray comprising: a gas permeable substrate for supporting a solid precursor, The gas permeable substrate has a perforation disposed adjacent the center of the gas permeable substrate; an outer ring disposed around an outer edge of the substrate and extending upwardly from the substrate, the outer ring Forming an interface with the lid of the container; and an inner ring disposed within the perforation, the inner ring being configured to form an interface with the lid of the container; an inlet disposed to pass the container a cover, the inlet being provided with a gas passing through the inner ring of the disk to an area below the disk; and an outlet disposed through the cover of the container to allow the solid precursor in the form of gas to flow out The capacity . The device of claim 1, wherein the disk comprises a plurality of disks stacked on each other, and an outer ring of each of the plurality of disks and an outer ring of another disk directly disposed on the disk Or with the lid of the container Forming an interface, and an inner ring of each of the plurality of disks is disposed to form an interface with an inner ring of another disk disposed directly on the disk or with the cover of the container, and wherein the area under the disk is a bit An area below a bottommost tray of the plurality of disks. The device of claim 2, wherein each of the outer ring and the inner ring includes an outwardly extending piece, and the outwardly extending piece is formed with an outer ring formed on another disk disposed directly on the disk. An interface is formed with each of the inner rings or a pocket formed in the lid of the container. The apparatus of any one of claims 1 to 3, further comprising: a temperature control unit configured to pass the inner ring of the disk to control a temperature within the container. The apparatus of claim 4, wherein the temperature control unit comprises at least one of a heater or a plurality of conduits configured to allow a heat transfer fluid to flow within the temperature control unit. The apparatus of any one of claims 1 to 3, wherein the container is made of stainless steel, a nichrome or quartz. The apparatus of any one of claims 1 to 3, further comprising a casing disposed around the container. The apparatus of claim 7, wherein the shell comprises an insulating material, a heater or a plurality of conduits configured to allow a heat transfer fluid to flow within the shell to be increased during use Or reducing a heat transfer from the container to control a temperature of the container. The apparatus of claim 7 further comprising an inner liner disposed between the outer casing and an outer surface of the container. The apparatus of claim 9, wherein the inner liner is made of quartz. The apparatus of any one of claims 1 to 3, wherein the gas permeable substrate comprises pores having a diameter of from about 25 to 150 microns. The apparatus of claim 11, wherein the gas permeable substrate comprises a quartz block or a stainless steel block. The apparatus of any one of claims 1 to 3, wherein the inner ring and the outer ring are made of stainless steel or quartz. The apparatus of any one of claims 1 to 3, further comprising a pressure monitor coupled to each of the disks to monitor a gas pressure within each of the disks. The device of any one of claims 1 to 3, further comprising a pressure monitor A controller that is coupled to the inlet and the outlet to monitor a pressure within the vessel. The apparatus of any one of claims 1 to 3, further comprising a heater coupled to the inlet and the outlet to control a temperature in the inlet and the outlet. The apparatus of any one of claims 1 to 3, further comprising a gas manifold disposed below the bottom and coupled to an end of the gas conduit, the gas manifold being configured to receive the gas manifold The gas is even spread around the gas at the bottom of the vessel. An apparatus for sublimating a solid precursor comprising: a container having a body, a cover and a removable bottom sealable to the body for coupling to the removable bottom The main body can seal the container; the first tray can be inserted into the container from a bottom of the container, the first tray comprises a gas permeable substrate, an inner wall and an outer wall, wherein the a gas permeable substrate for supporting a solid precursor and having a central opening formed through the substrate, the inner wall being disposed about the central opening of the substrate, the outer wall being disposed around an outer edge of the substrate, Wherein the inner wall forms an interface with the outer wall and the lid of the container to provide a hermetic seal between the first disc and the lid; an inlet disposed through the lid of the container and coupled to the lid An input channel to provide a gas to an area below the first disk, wherein the input channel passes through the central opening of the substrate and is at least partially defined by the inner wall of the first disk; and an outlet, the outlet Providing the cover through the container and positioned in a region generally above an area of the first disk between the inner wall and the outer wall of the first disk to permit the solid precursor in a gaseous form Can flow out of the container. The device of claim 18, further comprising: at least one second disk disposed under the first disk and having a gas permeable substrate, an inner wall and an outer wall, wherein the second disk The gas permeable substrate supports a solid precursor and has a central opening formed through the substrate of the second disk, the inner wall of the second disk surrounding the central opening of the substrate of the second disk Providing that the outer wall of the second disk is disposed around an outer edge of the base of the second disk, wherein the inner wall of the second disk and the outer wall and the inner wall and the outer wall of the first disk Forming an interface to provide a hermetic seal between the first disk and the second disk, and wherein the input channel passes through the central opening of the substrate of the second disk such that the first portion of the gas is provided The area below the disc is below the second disc. The apparatus of any one of claims 18 to 19, further comprising: a temperature control unit disposed in the container to control a temperature within the container.