FIELD

[001] The present disclosure relates to the field of processing solid chemistries.

BACKGROUND

[002] A variety of systems and methods can be used to process and store solid chemistries.

SUMMARY

[003] Solid chemistries delivery systems (e.g., a solid precursor material delivery system) have complex structures that improve delivery to a manufacturing tool. The delivery systems transfer heat to enhance the sublimation process. The solid chemistries delivery systems can have a control carrier gas flow.

[004] In some examples, the process of filling a solid delivery ampoule (e.g., a solid delivery ampoule used in a solid precursor material delivery system) with fill material (e.g., powder) involves removing a large diameter flanged lid and then removing the internal structure/trays inside a glovebox and manually measuring out and layering the solid back into the solid delivery ampoule.

[005] As vessels increase in size (e.g., a solid delivery ampoule), handling the fill material and trays can become increasingly difficult. For example, an increase in size of the vessel can include an increase in weight, besides the vessel becoming larger. The increase in weight and size can similarly make the vessels more difficult to handle as part of a solid chemistries delivery system.

[006] A new process that maximizes the fill weight and reduces total labor is needed to make delivery systems, such as solid chemistries delivery systems, manufacturable in high volumes.

[007] One way to reduce the increased vessel size is to increase the amount of solid chemistries can be packed into a given volume. By reducing the amount of volume required to hold a given amount of solid chemistries, a vessel with a smaller interior volume can be used. In some embodiments, the reduction in interior volume for the vessel can have a corresponding reduction in weight. Alternatively, the vessel size can remain constant and the amount of solid chemistries packed in the vessel can be increased. Either way, the required vessel size for a given amount of solid chemistries can be reduced, thereby reducing the demands placed on labor to process a given amount of solid chemistries.

[008] One way to accomplish the above is to introduce the fill material (e.g., a solid chemistry powder) through a single small diameter port on the top of the vessel. Apply vibration to the vessel directly to force the solid chemistry powder to move through-out the vessel. Allow enough time so that the powder becomes compacted in on itself increasing the bulk density of the powder and increasing the total fill weight by expelling excess air voids.

[009] In comparison to other processes, the process of the present disclosure can be used in manufacturing processes. One reason the present disclosure can be used in various manufacturing processes is due to the fill process not requiring removal of internal vessel components inside the glovebox.

[0010] The process of the present disclosure enables high bulk densities, which allow for higher fill weights thereby meeting an important customer need. The high bulk densities can be achieved by vibrating the vessel directly and/or indirectly to increase density and increase flowability of the powder. The fill time can be completed quickly with reduced voids in the powder, thereby providing superior results for a high fill weight (e.g., in a vapor draw application).

[0011 ] In some aspects, the techniques described herein relate to a system including: a vessel for containing a fill material; and a vibration source connected to the vessel, wherein the vibration source is configured to increase a bulk density of the fill material, wherein a fill material ratio includes a particle density of the fill material divided by the bulk density of the fill material after vibration, and wherein, after the vibration source increases the bulk density of the fill material, the fill material ratio can be more than 0.15, less than 0.75, or ranges from about 0.15 to about 0.75.

[0012] In some aspects, the techniques described herein relate to a system, wherein the fill material includes a solid precursor material.

[0013] In some aspects, the techniques described herein relate to a system, wherein the bulk density of the fill material can be more than 0.5, less 2, or range from about 0.5 to about 2.

[0014] In some aspects, the techniques described herein relate to a system, wherein the vibration source includes more than one vibration device.

[0015] In some aspects, the techniques described herein relate to a system, further including a funnel.

[0016] In some aspects, the techniques described herein relate to a system, wherein the funnel is connected to a top portion of the vessel, and wherein the funnel is configured to direct the fill material into the vessel.

[0017] In some aspects, the techniques described herein relate to a system, wherein the vessel includes a fill port.

[0018] In some aspects, the techniques described herein relate to a system, wherein the fill material enters the vessel through the fill port.

[0019] In some aspects, the techniques described herein relate to a vessel including: a sidewall and a bottom defining an interior volume; and a solid precursor material contained in the interior volume of the vessel, wherein a solid precursor material ratio includes a particle density of the solid precursor material divided by a bulk density of the solid precursor material after vibration, and wherein the solid precursor material ratio can be more than 0.15, less than 0.75, or ranges from about 0.15 to about 0.75.

[0020] In some aspects, the techniques described herein relate to a vessel, wherein the bulk density of the solid precursor material ranges can be more than 0.5, less 2, or range from about 0.5 to about 2.

[0021 ] In some aspects, the techniques described herein relate to a method including: filling an interior volume of a vessel with a fill material, wherein the interior volume of the vessel is defined by a sidewall and a bottom of the vessel; and vibrating the vessel, thereby increasing a bulk density of the fill material, wherein a fill material ratio includes a particle density of the fill material divided by the bulk density of the fill material after vibration, and wherein, after increasing the bulk density of the fill material, the fill material ratio ranges can be more than 0.15, less than 0.75, or ranges from about 0.15 to about 0.75.

[0022] In some aspects, the techniques described herein relate to a method, wherein the vibrating the vessel includes directly vibrating a body of the vessel.

[0023] In some aspects, the techniques described herein relate to a method, wherein the vibrating the vessel includes vibrating the vessel via one vibration device.

[0024] In some aspects, the techniques described herein relate to a method, wherein the vibrating the vessel includes vibrating the vessel via two or more vibration devices.

[0025] In some aspects, the techniques described herein relate to a method, wherein the vibrating the vessel includes continuously vibrating the vessel or applying vibration in a step-wise function.

[0026] In some aspects, the techniques described herein relate to a method, wherein the filing the interior volume of the vessel with the fill material includes introducing the fill material through a fill port of the vessel.

[0027] In some aspects, the techniques described herein relate to a method, wherein a diameter of the fill port ranges from about 0.25 inches to about 0.75 inches.

[0028] In some aspects, the techniques described herein relate to a method, wherein the vibrating the vessel reduces a void ratio of the vessel with the fill material.

[0029] In some aspects, the techniques described herein relate to a method, wherein the fill material includes a solid precursor material.

[0030] In some aspects, the techniques described herein relate to a method, wherein the bulk density of the fill material can be more than 0.5, less 2, or range from about 0.5 to about 2. DRAWINGS

[0031 ] Some embodiments of the disclosure are herein described, by way of example only, with reference to the accompanying drawings. With specific reference now to the drawings in detail, it is stressed that the embodiments shown are by way of example and for purposes of illustrative discussion of embodiments of the disclosure. In this regard, the description taken with the drawings makes apparent to those skilled in the art how embodiments of the disclosure may be practiced.

[0032] FIG. 1 A depicts a non-limiting embodiment of a vessel prior to vibration.

[0033] FIG. 1 B depicts a non-limiting embodiment of a vessel post-vibration.

[0034] FIG. 2 depicts a non-limiting embodiment of the system described herein.

[0035] FIG. 3 shows a flowchart according to some of the embodiments of the methods according to the present disclosure.

DETAILED DESCRIPTION

[0036] Among those benefits and improvements that have been disclosed, other objects and advantages of this disclosure will become apparent from the following description taken in conjunction with the accompanying figures. Detailed embodiments of the present disclosure are disclosed herein; however, it is to be understood that the disclosed embodiments are merely illustrative of the disclosure that may be embodied in various forms. In addition, each of the examples given regarding the various embodiments of the disclosure which are intended to be illustrative, and not restrictive.

[0037] Throughout the specification and claims, the following terms take the meanings explicitly associated herein, unless the context clearly dictates otherwise. The phrases "in one embodiment," “in an embodiment,” and "in some embodiments" as used herein do not necessarily refer to the same embodiment(s), though it may. Furthermore, the phrases "in another embodiment" and "in some other embodiments" as used herein do not necessarily refer to a different embodiment, although it may. All embodiments of the disclosure are intended to be combinable without departing from the scope or spirit of the disclosure.

[0038] As used herein, the term "based on" is not exclusive and allows for being based on additional factors not described, unless the context clearly dictates otherwise. In addition, throughout the specification, the meaning of "a," "an," and "the" include plural references. The meaning of "in" includes "in" and "on."

[0039] As used herein, “bulk density” (which can also be called apparent density or volumetric density) is the ratio of the mass of the fill material divided by the total volume. Unless otherwise provided herein, the units of bulk density are g/cm ³ .

[0040] As used herein, “void ratio” is the ratio of the volume of voids to the volume of solids.

[0041 ] Solid chemistry delivery systems can have complex structures to transfer heat to enhance the sublimation process that allows delivery to a manufacturing tool.

[0042] In some examples, the process of filling solid delivery vessels with fil material involves removing a large diameter flanged lid and then removing the internal structure/trays inside a glovebox and manually measuring out and layering the solid back into the vessel. The larger the vessel the more exponential the process of the present disclosure can be impacted man-power wise.

[0043] For a fill weight of a particular range, the process of the present disclosure reduces total labor required to make delivery systems, thereby allowing the delivery systems to be manufacturable in high volumes.

[0044] In some embodiments, the process of the present disclosure includes introducing the fill material (e.g. a solid chemistry powder) through a single small diameter port on the top of the vessel. The present disclosure can include applying vibration to the vessel directly and/or indirectly to force the fill material to move throughout the vessel. In some embodiments, vibration may be applied only indirectly to the vessel. An amount of time can lapse so that the fill material becomes compacted in on itself increasing the bulk density of the powder and optimizing the total fill weight. In some embodiments, the amount of time for the fill material to be compacted can be greater than one minute, less than 10 minutes, or range from one minute to ten minutes. In some embodiments, the amount of time for the fill material to be compacted can be greater than one minute, less than 120 minutes, or range from one minute to 120 minutes.

[0045] In some embodiments, the methods of the present disclosure are used on fill materials (e.g., high density fill materials), including solid chemistry powder (e.g., solid chemistry powder of AlCh or M0O2CI2) to achieve a higher fill weight and decrease overall cost of ownership as per required from the customer year after year.

[0046] The present disclosure includes attaching a vibration device directly (as well as indirectly) to the body of the vessel to increase the movement of the powder, driving excess air voids out of the vessel and maximizing the bulk density in the powder.

[0047] FIG. 1 A depicts a system 100 with a vessel 1 10 filled with a fill material 120 in a pre-vibration state. A fill line 130 indicates a fill level of the fill material 120 in the vessel 110 in a pre-vibration state. In some examples, the process of filling the vessel 110 with the fill material 120 does not include vibration. Consequently, the fill material 120 includes more air voids within the fill material 120 as compared to a system (e.g., the system 100’ in FIG. 1 B) where the vessel is vibrated. The bulk density of the system 100 can be increased by decreasing the number of air voids in the fill material 120. Accordingly, more fill material 120 can fill the volume of the vessel 110 by reducing the air voids within the fill material 120. That is, the void ratio of the fill material 120 can be reduced and more fill material 120 can be added to the vessel 110.

[0048] In some embodiments, the fill material 120 comprises, consists of, or consists essentially of at least one of hafnium chloride (HfCk), zirconium chloride (ZrCk), indium trichloride, indium monochloride, aluminum trichloride, titanium iodide, tungsten carbonyl, Ba(DPM)2, bis dipivaloyl methanato strontium (Sr(DPM)2), TiO(DPM)2, tetra dipivaloyl methanato zirconium (Zr(DPM)4), decaborane, octadecaborane, phosphorous, arsenic, precursors incorporating alkyl-amidinate ligands, organometallic precursors, tetrakis (dimethylamino) titanium (TDMAT), pentakis (dimethylamino) tantalum (PDMAT), pentakis (ethylmethylamino) tantalum (PEMAT), tetrakisdimethylaminozirconium (Zr(NMe2)4), xenon difluoride (XeF2), xenon tetrafluoride (XeF^, xenon hexafluoride (XeFe), or any combination thereof.

[0049] In some embodiments, the fill material 120 comprises, consists of, or consists essentially of at least one of decaborane, hafnium tetrachloride, zirconium tetrachloride, indium trichloride, metalorganic p-diketonate complexes, , cyclopentadienylcycloheptatrienyl-titanium (CpTiCht), aluminum trichloride, titanium iodide, cyclooctatetraenecyclo-pentadienyltitanium, biscyclopentadienyltitaniumdiazide, , trimethyl indium tungsten carbonyl, or any combination thereof.

[0050] In some embodiments, the fill material 120 comprises, consists of, or consists essentially of at least one of elemental phosphorus, decaborane, gallium halides, indium halides, antimony halides, arsenic halides, gallium halides, aluminum iodide, titanium iodide, Mo02CI2, MoOCI4, MoCI5, WCI5, W0CI4, WCI6, cyclopentadienylcycloheptatrienyltitanium (CpTiCht), cyclooctatetraenecyclopenta-dienyltitanium, biscyclopentadienyltitanium-diazide, ln(CH3)2(hfac), dibromomethyl stibine, tungsten carbonyl, metalorganic - diketonate complexes, metalorganic alkoxide complexes, metalorganic carboxylate complexes, metalorganic aryl complexes, metalorganic amido complexes, or any combination thereof. In some embodiments, the fill material 120 comprises, consists of, or consists essentially of at least one of Mo02CI2, MoOCI4, WO2CI2, WOCI4, or any combination thereof.

[0051 ] FIG. 1 B depicts a system 100’ with a vessel 110’ filled with a fill material 120’ in a post-vibration state. A fill line 130’ indicates a fill level of the fill material 120’ in the vessel 1 10’ in a post-vibration state. The amount of the fill material 120 in FIG. 1 A can be the same as the 120’ in FIG. 1 B. The fill line 130’ is lowered due to, at least in part, the reduction in air voids of the fill material 120’.

[0052] The vessel 110’ can be repeatedly filled with the fill material 120’ and vibrated. In this way, moving the fill line 130’ up the vessel 1 10’. For example, the vessel 110’ can be filled and vibrated until the vessel 110’ is full of the fill material 120’. When the vessel 1 10’ is full of the fill material 120’, the fill line 130’ will be at the top of the vessel 1 10’. In some embodiments, the void ratio for the vessel 110’ with the fill material 120’ can be more than 50%, less than 80%, or range from 50% to 80%.

[0053] FIG. 2 depicts a non-limiting embodiment of the system 200 described herein. For simplicity of this Specification, features of the system 200 that have been previously described respective of FIG. 1 A and FIG. 1 B will not be redescribed in additional detail unless specifically indicated otherwise. The system 200 includes a vessel 210 with a fill line 230 of fill material. The vessel 210 has a sidewall 212, a bottom 214, and a top 216. The sidewall 212 and the bottom 214 define an interior volume 218 of the vessel 210. In some embodiments, the system 200 includes a vibration source 240 connected to the vessel 210. In some embodiments, the vibration source 240 is connected to an attachment mechanism 250. In some embodiments, the attachment mechanism 250 attaches the vibration source 240 to the vessel 210. In some embodiments, the vessel 210 includes a fill port 260. In some embodiments, the fill material enters the vessel 210 through the fill port 260. In some embodiments, the system 200 includes a funnel 270 to assist in filling the vessel 210 through the fill port 260 with a fill material. In some embodiments, the fill material is added to the vessel 210 through fill port 260 without the use of the funnel 270.

[0054] In some embodiments, the vibration source 240 can increase a bulk density of the fill material in the vessel 210. A fill material ratio can be defined as a particle density of the fill material divided by the bulk density of the fill material after vibration.

[0055] In some embodiments, the vibration source 240 vibrates the vessel 210 by continuously vibrating the vessel 210 or applying vibration in a step-wise function. The vibration source 240 may vary the frequency and amplitude of vibration. For example, continuously vibrating the vessel 210 at a constant frequency and amplitude. Alternatively, vibrating the vessel 210 may include varying one, or both, of the frequency and amplitude.

[0056] In some embodiments, a particle density of the fill material can be more than 0.5, less 2, or range from about 0.5 to about 2. In some embodiments, a bulk density of the fill material, in a pre-vibration state, can range from can be more than 0.1 , less 0.5, or range from about 0.1 to about 0.5. In some embodiments, a bulk density of the fill material, in a post-vibration state, can be more than 0.5, less 2, or range from about 0.5 to about 2. In some embodiments, a bulk density of the fill material, in a post-vibration state, can be more than 1 , less than 5, or range from about 1 to 5.

[0057] In some embodiments, after the vibration source 240 increases the bulk density of the fill material, the fill material ratio can be more than 0.15, less than 0.75, or ranges from about 0.15 to about 0.75.

[0058] In some embodiments, the vibration source 240 includes more than one vibration device. For example, the vibration source 240 may include two vibration devices. In some embodiments, when the system 200 includes more than one vibration device for the vibration source 240, the vibration devices may be the same or substantially similar. In some embodiments, when the system 200 includes more than one vibration device for the vibration source 240, the vibration devices may differ from one another. For example, one vibration device may vibrate the vessel 210 directly and another vibration device may vibrate the vessel 210 indirectly.

[0059] In some embodiments, the vibration source 240 is not connected via the attachment mechanism 250 to the vessel 210. For example, in some embodiments, the vibration source 240 can be a vibrating surface that the vessel 210 is placed on and/or adjacent to.

[0060] In some embodiments, a diameter of the fill port 260 ranges from about 0.25 inches to about 0.75 inches. In some embodiments, the vessel 210 can include more than one fill port 260. For example, the vessel 210 can include three fill ports 260. In some embodiments, the fill port 260 is located on a side of the vessel 210. In some embodiments, when the vessel 210 includes more than one fill port 260, one fill port 260 can be located on top 216 of the vessel 210 and another fill port 260 can be located on a side of the vessel 210. In some embodiments, the fill material is added to the vessel 210 through fill port 260 without the use of the funnel 270.

[0061 ] In some embodiments, the funnel 270 is connected to the vessel 210. In some embodiments, the funnel 270 is connected at the top 216 of the vessel 210. In some embodiments, the funnel 270 is connected to a side of the vessel 210. The funnel 270 can direct the fill material into the vessel 210. In some embodiments, the funnel 270 is not connected to the vessel 210. In some embodiments, the funnel 270 remains stationary as new vessels (multiples of the vessel 210) are brought underneath the funnel 270. The funnel 270 can then be aligned with the fill port 260 and fill material added to the vessel 210.

[0062] In some embodiments, the system 200 includes more than one funnel 270. In some embodiments, more than one funnel 270 is connected to a single fill port 260. In some embodiments, the system includes more than one fill port 260 and more than one funnel 270. In some embodiments, a first funnel 270 can be connected to a first fill port 260 on a side of the vessel 210, and a second funnel 270 can be connected to the top 216 of the vessel 210. In some embodiments, a first funnel 270 can be connected to a first fill port 260 on a side of the vessel 210, and a second funnel 270 can be connected on a side of the vessel 210. In some embodiments, a first funnel 270 can be connected to a first fill port 260 on the top 216 of the vessel 210, and a second funnel 270 can be connected to the top 216 of the vessel 210.

[0063] FIG 3. shows a flowchart according to some of the embodiments of the methods according to the present disclosure. The system used in the method 300 can be any of the embodiments described herein (e.g., the system 200). The method 300 includes filling 310 an interior volume of a vessel with a fill material, wherein the interior volume of the vessel is defined by a sidewall and a bottom of the vessel; and vibrating 320 the vessel, thereby increasing a bulk density of the fill material. [0064] In some embodiments, the vibrating 320 the vessel includes directly vibrating a body of the vessel. In some embodiments, the vibrating the vessel includes vibrating the vessel via one vibration device. In some embodiments, the vibrating the vessel includes vibrating the vessel via two or more vibration devices. In some embodiments, the vibrating the vessel includes continuously vibrating the vessel or applying vibration in a step-wise function. In some embodiments, the vibrating 320 the vessel reduces a void ratio of the vessel with the fill material. In some embodiments, by vibrating the vessel, a fill weight of the vessel can increase by 5% to 30% relative to a fill weight of a vessel which is not subjected to vibrating.

[0065] In some embodiments, the filing 310 the interior volume of the vessel with the fill material comprises introducing the fill material through a fill port of the vessel.

[0066] ASPECTS

[0067] Various Aspects are described below. It is to be understood that any one or more of the features recited in the following Aspect(s) can be combined with any one or more other Aspect(s).

[0068] Aspect 1 . A system comprising: a vessel for containing a fill material; and a vibration source connected to the vessel, wherein the vibration source is configured to increase a bulk density of the fill material, wherein a fill material ratio comprises a particle density of the fill material divided by the bulk density of the fill material after vibration, and wherein, after the vibration source increases the bulk density of the fill material, the fill material ratio ranges from about 0.15 to about 0.75.

[0069] Aspect 2. The system of Aspect 1 , wherein the fill material comprises a solid precursor material.

[0070] Aspect 3. The system of Aspect 1 or Aspect 2, wherein the bulk density of the fill material ranges from about 0.5 to about 2.

[0071 ] Aspect 4. The system as in any of the preceding Aspects, wherein the vibration source comprises more than one vibration device. [0072] Aspect 5. The system as in any of the preceding Aspects, further comprising a funnel.

[0073] Aspect 6. The system of Aspect 5, wherein the funnel is connected to a top portion of the vessel, and wherein the funnel is configured to direct the fill material into the vessel.

[0074] Aspect 7. The system as in any of the preceding Aspects, wherein the vessel comprises a fill port.

[0075] Aspect 8. The system of Aspect 7, wherein the fill material enters the vessel through the fill port.

[0076] Aspect 9. A vessel comprising: a sidewall and a bottom defining an interior volume; and a solid precursor material contained in the interior volume of the vessel, wherein a solid precursor material ratio comprises a particle density of the solid precursor material divided by a bulk density of the solid precursor material after vibration, and wherein the solid precursor material ratio ranges from about 0.15 to about 0.75.

[0077] Aspect 10. The vessel of Aspect 9, wherein the bulk density of the solid precursor material ranges from about 0.5 to about 2.

[0078] Aspect 1 1 . A method comprising: filling an interior volume of a vessel with a fill material, wherein the interior volume of the vessel is defined by a sidewall and a bottom of the vessel; and vibrating the vessel, thereby increasing a bulk density of the fill material, wherein a fill material ratio comprises a particle density of the fill material divided by the bulk density of the fill material after vibration, and wherein, after increasing the bulk density of the fill material, the fill material ratio ranges from about 0.15 to about 0.75.

[0079] Aspect 12. The method of Aspect 1 1 , wherein the vibrating the vessel comprises directly vibrating a body of the vessel.

[0080] Aspect 13. The method of Aspect 1 1 or Aspect 12, wherein the vibrating the vessel comprises vibrating the vessel via one vibration device.

[0081 ] Aspect 14. The method as in any of the preceding Aspects, wherein the vibrating the vessel comprises vibrating the vessel via two or more vibration devices. [0082] Aspect 15. The method as in any of the preceding Aspects, wherein the vibrating the vessel comprises continuously vibrating the vessel or applying vibration in a step-wise function.

[0083] Aspect 16. The method as in any of the preceding Aspects, wherein the filing the interior volume of the vessel with the fill material comprises introducing the fill material through a fill port of the vessel.

[0084] Aspect 17. The method of Aspect 16, wherein a diameter of the fill port ranges from about 0.25 inches to about 0.75 inches.

[0085] Aspect 18. The method as in any of the preceding Aspects, wherein the vibrating the vessel reduces a void ratio of the vessel with the fill material.

[0086] Aspect 19. The method as in any of the preceding Aspects, wherein the fill material comprises a solid precursor material.

[0087] Aspect 20. The method as in any of the preceding Aspects, wherein the bulk density of the fill material ranges from about 0.5 to about 2.

[0088] It is to be understood that changes may be made in detail, especially in matters of the construction materials employed and the shape, size, and arrangement of parts without departing from the scope of the present disclosure. This Specification and the embodiments described are examples, with the true scope and spirit of the disclosure being indicated by the claims that follow.