Vibratory filling process for solid chemical substances

Abstract

A system including a container for accommodating a filling material and a vibration source connected to the container. The vibration source can increase the bulk density of the filling material. The ratio of the filling material can be defined as the particle density of the filling material divided by the bulk density of the filling material after vibration. After the vibration source increases the bulk density of the filling material, the ratio of the filling material can be in the range of about 0.15 to about 0.75.

Description

Technical Field

[0001] The present disclosure relates to the field of processing solid chemical substances.

Background Art

[0002] Various systems and methods can be used to process and store solid chemical substances.

Summary of the Invention

[0003] A solid chemical substance delivery system (e.g., a solid precursor material delivery system) has a complex structure that improves delivery to a manufacturing tool. The delivery system transfers heat to enhance the sublimation process. The solid chemical substance delivery system can have a controlled carrier gas flow.

[0004] 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 a filling material (e.g., powder) involves removing a large-diameter flanged lid, then removing an internal structure / tray within a glove box, manually measuring the solid, layering it, and returning it to the solid delivery ampoule.

[0005] As the size of the container (e.g., a solid delivery ampoule) increases, handling of the filling material and tray can become increasingly difficult. For example, an increase in the size of the container can include an increase in weight in addition to the container becoming larger. Similarly, the increase in weight and size can make it more difficult to handle the container as part of a solid chemical substance delivery system.

[0006] To enable the manufacture of delivery systems such as solid chemical substance delivery systems in large volumes, a new process is needed that maximizes the filling weight and reduces the total labor.

[0007] One way to reduce the increased container size is to increase the amount of solid chemical that can be packed into a given volume. By reducing the volume amount required to hold a given amount of solid chemical, a container with a smaller internal volume can be used. In some embodiments, the reduction in the internal volume of the container may have a corresponding weight reduction. Alternatively, the container size can be kept constant and the amount of solid chemical packed into the container can be increased. Either way, the container size required for a given amount of solid chemical can be reduced, thereby reducing the labor-intensive requirements for processing a given amount of solid chemical.

[0008] One way to achieve the above is to introduce a packing material (e.g., powder of solid chemical) through a single small-diameter port at the top of the container. Direct vibration is applied to the container to move the powder of the solid chemical through the container. Allow sufficient time so that the powder compresses itself to increase the bulk density of the powder and expel excess air bubbles, thereby increasing the total filling weight.

[0009] Compared 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 filling process not requiring the removal of internal container components within a glove box.

[0010] The process of the present disclosure enables a high bulk density and a higher filling weight, thereby meeting the important customer needs. The high bulk density can be achieved by directly and / or indirectly vibrating the container to increase the density of the powder and enhance its fluidity. The filling time can be quickly completed by reducing the voids in the powder, thereby resulting in excellent results for a high filling weight (e.g., in vapor suction applications).

[0011] In some aspects, the technology described herein relates to a system comprising a container for containing a packing material and a vibration source connected to the container, the vibration source being configured to increase the bulk density of the packing material, the ratio of the packing material including the particle density of the packing material divided by the bulk density of the packing material after vibration, and after the vibration source increases the bulk density of the packing material, the ratio of the packing material can be greater than 0.15, less than 0.75, or in the range of about 0.15 to about 0.75.

[0012] In some aspects, the technology described herein relates to a system wherein the packing material includes a solid precursor material.

[0013] In some aspects, the technology described herein relates to a system wherein the bulk density of the packing material can be greater than 0.5, less than 2, or in the range of about 0.5 to about 2.

[0014] In some aspects, the technology described herein relates to a system wherein the vibration source includes two or more vibration devices.

[0015] In some aspects, the technology described herein relates to a system further comprising a funnel.

[0016] In some aspects, the technology described herein relates to a system wherein the funnel is connected to the upper part of the container and is configured to guide the packing material into the container.

[0017] In some aspects, the technology described herein relates to a system wherein the container includes a filling port.

[0018] In some aspects, the technology described herein relates to a system wherein the packing material enters the container through the filling port.

[0019] In some aspects, the technology described herein relates to a container that includes sidewalls and a bottom that define an internal volume, and a solid precursor material contained within the internal volume of the container, where the ratio of the solid precursor material includes the particle density of the solid precursor material divided by the bulk density of the solid precursor material after vibration, and the ratio of the solid precursor material can be greater than 0.15, less than 0.75, or in the range of about 0.15 to about 0.75.

[0020] In some aspects, the technology described herein relates to a container where the bulk density range of the solid precursor material can be greater than 0.5, less than 2, or in the range of about 0.5 to about 2.

[0021] In some aspects, the technology described herein relates to a method that includes filling the internal volume of a container with a filling material, where the internal volume of the container is defined by the sidewalls and bottom of the container, and vibrating the container to thereby increase the bulk density of the filling material, where the ratio of the filling material includes the particle density of the filling material divided by the bulk density of the filling material after vibration, and after increasing the bulk density of the filling material, the range of the ratio of the filling material can be greater than 0.15, less than 0.75, or in the range of about 0.15 to about 0.75.

[0022] In some aspects, the technology described herein relates to a method where vibrating the container includes directly vibrating the body of the container.

[0023] In some aspects, the technology described herein relates to a method where vibrating the container includes vibrating the container via one vibration device.

[0024] In some aspects, the technology described herein relates to a method where vibrating the container includes vibrating the container via two or more vibration devices.

[0025] In some embodiments, the techniques described herein relate to a method, wherein vibrating the container comprises continuously vibrating the container or applying vibrations in stages.

[0026] In some embodiments, the techniques described herein relate to a method, wherein filling the internal volume of the container with a filling material comprises introducing the filling material through a filling port of the container.

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

[0028] In some embodiments, the techniques described herein relate to a method, wherein vibrating the container reduces the porosity of the container containing the filling material.

[0029] In some embodiments, the techniques described herein relate to a method, wherein the filling material comprises a solid precursor material.

[0030] In some embodiments, the techniques described herein relate to a method, wherein the bulk density of the filling material can be greater than 0.5, less than 2, or in the range of about 0.5 to about 2.

[0031] Some embodiments of the present disclosure are described herein by way of example only with reference to the accompanying drawings. Here, when referring specifically to the drawings in detail, it is emphasized that the embodiments shown are for illustrative purposes and are for an exemplary explanation of the embodiments of the present disclosure. In this regard, the description made with the use of the drawings will clarify to those skilled in the art how the embodiments of the present disclosure can be implemented.

Brief Description of the Drawings

[0032]

Figure 1A

Figure 1B

Figure 2

Figure 3

[0033] Among these disclosed advantages and improvements, other objects and advantages of the present disclosure will become apparent from the following description in conjunction with the accompanying drawings. Although detailed embodiments of the present disclosure are disclosed herein, it should be understood that the disclosed embodiments are merely exemplary of the present disclosure, which can be embodied in various forms. Furthermore, each of the examples given with respect to the various embodiments of the present disclosure is intended to be illustrative and not limiting.

[0034] Throughout the specification and the claims, the following terms take the meanings explicitly associated herein unless the context clearly indicates otherwise. The phrases "in one embodiment," "in an embodiment," and "in some embodiments," when used herein, do not necessarily refer to the same embodiment, but may. Further, the phrases "in another embodiment" and "in some other embodiments," when used herein, do not necessarily refer to different embodiments, but may. It is intended that all embodiments of the present disclosure be combinable without departing from the scope or spirit of the present disclosure.

[0035] As used herein, the term "based on" is not exclusive and allows for being based on additional factors not recited, unless the context clearly dictates otherwise. Further, throughout the specification, the meanings of "a," "an," and "the" include plural referents. The meaning of "in" includes "in" and "on."

[0036] As used herein, "bulk density" (which may also be referred to as apparent density or volume density) is the ratio of the mass of the filling material divided by the total volume. Unless otherwise provided herein, the unit of bulk density is g / cm 3 is.

[0037] As used herein, "porosity" is the ratio of the volume of voids to the volume of solids.

[0038] A solid chemical delivery system may have a complex structure for transferring heat to enhance the sublimation process that enables delivery to a manufacturing tool.

[0039] In some examples, the process of filling a solid delivery container with a filling material includes removing a large-diameter flanged lid, then removing the internal structure / tray within the glove box, manually measuring the solid, layering it, and returning it to the container. The larger the container, the more acutely the process of the present disclosure may be affected from a manpower perspective.

[0040] For a specific range of filling weights, the process of the present disclosure reduces the total labor required to fabricate the delivery system, thereby enabling the delivery system to be manufactured in large volumes.

[0041] In some embodiments, the process of the present disclosure includes introducing a filling material (e.g., a powder of a solid chemical) through a single small-diameter port at the top of the container. The present disclosure may include applying vibration directly and / or indirectly to the container to move the filling material throughout the container. In some embodiments, the vibration may be applied only indirectly to the container. An amount of time may elapse such that the filling material is compressed by itself to increase the bulk density of the powder and optimize the total filling weight. In some embodiments, the amount of time the filling material is compressed may be greater than 1 minute, less than 10 minutes, or in the range of 1 minute to 10 minutes. In some embodiments, the amount of time the filling material is compressed may be greater than 1 minute, less than 120 minutes, or in the range of 1 minute to 120 minutes.

[0042] In some embodiments, the methods of the present disclosure are used with a packing material (e.g., a high-density packing material) that includes a powder of a solid chemical substance (e.g., a powder of a solid chemical substance such as AlCl3 or MoO2Cl2) to achieve a higher packing weight and reduce the overall cost of ownership, as requested by customers each year.

[0043] The present disclosure includes directly (and indirectly) attaching a vibration device to the body of a container to increase the movement of the powder, expel excess air bubbles from the container, and maximize the bulk density of the powder.

[0044] FIG. 1A shows a system 100 having a container 110 filled with a packing material 120 in a state before vibration. A filling line 130 indicates the filling level of the packing material 120 in the container 110 in a state before vibration. In some examples, the process of filling the container 110 with the packing material 120 does not include vibration. As a result, the packing material 120 contains more air bubbles therein compared to a system in which the container vibrates (e.g., system 100' in FIG. 1B). The bulk density of the system 100 can be increased by reducing the number of air bubbles in the packing material 120. Thus, more of the packing material 120 can fill the volume of the container 110 by reducing the air bubbles in the packing material 120. That is, the porosity of the packing material 120 can be reduced, and more of the packing material 120 can be added to the container 110.

[0045] In some embodiments, the filling material 120 comprises, consists of, or consists essentially of at least one of hafnium chloride (HfCl4), zirconium chloride (ZrCl4), indium trichloride, indium monochloride, aluminum trichloride, titanium iodide, tungsten carbonyl, Ba(DPM)2, strontium bis(dipivaloylmethanato) (Sr(DPM)2), TiO(DPM)2, zirconium tetrakis(dipivaloylmethanato) (Zr(DPM)4), decaborane, octadecaborane, phosphorus, arsenic, a precursor incorporating an alkylamidinato ligand, an organometallic precursor, tetrakis(dimethylamino)titanium (TDMAT), pentakis(dimethylamino)tantalum (PDMAT), pentakis(ethylmethylamino)tantalum (PEMAT), tetrakis(dimethylamino)zirconium (Zr(NMe2)4), xenon difluoride (XeF2), xenon tetrafluoride (XeF4), xenon hexafluoride (XeF6), or any combination thereof.

[0046] In some embodiments, the filling material 120 comprises, consists of, or consists essentially of at least one of decaborane, hafnium tetrachloride, zirconium tetrachloride, indium trichloride, a metal-organic β-diketonate complex, cyclopentadienylcycloheptatrienyl-titanium (CpTiCht), aluminum trichloride, titanium iodide, cyclooctatetraenylcyclo-pentadienyltitanium, biscyclopentadienyltitanium diazide, trimethylindium tungsten carbonyl, or any combination thereof.

[0047] In some embodiments, the filling 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, MoO2Cl2, MoOCl4, MoCl5, WCl5, WOCl4, WCl6, cyclopentadienylcycloheptatrienyltitanium (CpTiCht), cyclooctatetraene cyclopentadienyltitanium, biscyclopentadienyltitanium-diazide, In(CH3)2(hfac), dibromomethylstibine, tungsten carbonyl, metal-organic β-diketonate complexes, metal-organic alkoxide complexes, metal-organic carboxylate complexes, metal-organic aryl complexes, metal-organic amide complexes, or any combination thereof. In some embodiments, the filling material 120 comprises, consists of, or consists essentially of at least one of MoO2Cl2, MoOCl4, WO2Cl2, WOCl4, or any combination thereof.

[0048] Figure 1B shows a system 100' having a container 110' filled with a filling material 120' in a post-vibration state. The filling line 130' indicates the filling level of the filling material 120' within the container 110' in the post-vibration state. The amount of the filling material 120 in Figure 1A can be the same as 120' in Figure 1B. The filling line 130' decreases at least in part due to the reduction of air bubbles in the filling material 120'.

[0049] The container 110' can be repeatedly filled with the filling material 120' and vibrated. In this way, the filling line 130' is moved above the container 110'. For example, the container 110' can be filled and vibrated until the container 110' is filled with the filling material 120'. When the container 110' is filled with the filling material 120', the filling line 130' is at the upper part of the container 110'. In some embodiments, the porosity of the container 110' with the filling material 120' can be greater than 50%, less than 80%, or in the range of 50% to 80%.

[0050] Figure 2 shows a non-limiting embodiment of system 200 described herein. For the sake of simplicity of this specification, the features of system 200 previously described in each of FIGS. 1A and 1B will not be re-described in further detail unless otherwise specifically stated. System 200 includes a container 210 having a filling line 230 for a filling material. Container 210 has a side wall 212, a bottom 214, and an upper portion 216. Side wall 212 and bottom 214 define an internal volume 218 of container 210. In some embodiments, system 200 includes a vibration source 240 connected to container 210. In some embodiments, vibration source 240 is connected to an attachment mechanism 250. In some embodiments, attachment mechanism 250 attaches vibration source 240 to container 210. In some embodiments, container 210 includes a filling port 260. In some embodiments, the filling material enters container 210 through filling port 260. In some embodiments, system 200 includes a funnel 270 to assist in filling container 210 with the filling material through filling port 260. In some embodiments, the filling material is added to container 210 through filling port 260 without using funnel 270.

[0051] In some embodiments, vibration source 240 can increase the bulk density of the filling material within container 210. The ratio of the filling material can be defined as the particle density of the filling material divided by the bulk density of the filling material after vibration.

[0052] In some embodiments, vibration source 240 vibrates container 210 by continuously vibrating container 210 or applying vibration in stages. Vibration source 240 can vary the vibration frequency and vibration amplitude. For example, container 210 is continuously vibrated at a constant vibration frequency and vibration amplitude. Alternatively, vibrating container 210 may include changing one or both of the vibration frequency and vibration amplitude.

[0053] In some embodiments, the particle density of the filling material can be greater than 0.5, less than 2, or in the range of about 0.5 to about 2. In some embodiments, the bulk density of the filling material in the state before vibration can be greater than 0.1, less than 0.5, or in the range of about 0.1 to about 0.5. In some embodiments, the bulk density of the filling material in the state after vibration can be greater than 0.5, less than 2, or in the range of about 0.5 to about 2. In some embodiments, the bulk density of the filling material in the state after vibration can be greater than 1, less than 5, or in the range of about 1 to 5.

[0054] In some embodiments, after the vibration source 240 increases the bulk density of the filling material, the ratio of the filling material can be greater than 0.15, less than 0.75, or in the range of about 0.15 to about 0.75.

[0055] In some embodiments, the vibration source 240 includes two or more vibration devices. For example, the vibration source 240 may include two vibration devices. In some embodiments, when the system 200 includes two or more vibration devices for the vibration source 240, the vibration devices may be the same or substantially the same. In some embodiments, when the system 200 includes two or more vibration devices for the vibration source 240, the vibration devices may be different from each other. For example, one vibration device may directly vibrate the container 210, and another vibration device may indirectly vibrate the container 210.

[0056] In some embodiments, the vibration source 240 is not connected to the container 210 via the attachment mechanism 250. For example, in some embodiments, the vibration source 240 may be present on a vibration surface on which and / or adjacent to the container 210 is disposed.

[0057] In some embodiments, the diameter of the filling port 260 ranges from about 0.25 inches to about 0.75 inches. In some embodiments, the container 210 may include two or more filling ports 260. For example, the container 210 may include three filling ports 260. In some embodiments, the filling port 260 is installed on the side surface of the container 210. In some embodiments, when the container 210 includes two or more filling ports 260, one filling port 260 may be installed on the upper portion 216 of the container 210, and another filling port 260 may be installed on the side surface of the container 210. In some embodiments, the filling material is added to the container 210 through the filling port 260 without using the funnel 270.

[0058] In some embodiments, the funnel 270 is connected to the container 210. In some embodiments, the funnel 270 is connected to the upper portion 216 of the container 210. In some embodiments, the funnel 270 is connected to the side surface of the container 210. The funnel 270 can guide the filling material into the container 210. In some embodiments, the funnel 270 is not connected to the container 210. In some embodiments, when a new container (a multiple of the container 210) is brought under the funnel 270, the funnel 270 remains stationary. Then, the funnel 270 can be aligned with the filling port 260, and the filling material can be added to the container 210.

[0059] In some embodiments, system 200 includes two or more funnels 270. In some embodiments, two or more funnels 270 are connected to a single filling port 260. In some embodiments, the system includes two or more filling ports 260 and two or more funnels 270. In some embodiments, the first funnel 270 may be connected to the first filling port 260 on the side of the container 210, and the second funnel 270 may be connected to the upper portion 216 of the container 210. In some embodiments, the first funnel 270 may be connected to the first filling port 260 on the side of the container 210, and the second funnel 270 may be connected to the side of the container 210. In some embodiments, the first funnel 270 may be connected to the first filling port 260 in the upper portion 216 of the container 210, and the second funnel 270 may be connected to the upper portion 216 of the container 210.

[0060] Figure 3 shows a flowchart according to some embodiments of a method according to the present disclosure. The system used in method 300 can be any of the embodiments described herein (e.g., system 200). Method 300 includes filling 310 the internal volume of a container with a filling material, where the internal volume of the container is defined by the sidewalls and bottom of the container, and vibrating (320) the container, thereby increasing the bulk density of the filling material.

[0061] In some embodiments, vibrating 320 the container includes directly vibrating the body of the container. In some embodiments, vibrating the container includes vibrating the container via one vibration device. In some embodiments, vibrating the container includes vibrating the container via two or more vibration devices. In some embodiments, vibrating the container includes continuously vibrating the container or applying vibrations in stages. In some embodiments, vibrating 320 the container reduces the porosity of the container containing the filling material. In some embodiments, by vibrating the container, the filling weight of the container can increase by 5% to 30% relative to the filling weight of a container not subjected to vibration.

[0062] In some embodiments, filling the internal volume of the container with the filling material 310 includes introducing the filling material through a filling port of the container.

[0063] Aspect The following various aspects are described. It should be understood that any one or more of the features described in the following aspects can be combined with any one or more of the other aspects.

[0064] Aspect 1. A system comprising a container for containing a filling material and a vibration source connected to the container, the vibration source being configured to increase the bulk density of the filling material, the ratio of the filling material including that obtained by dividing the particle density of the filling material by the bulk density of the filling material after vibration, and the vibration source being such that after increasing the bulk density of the filling material, the ratio of the filling material is in the range of about 0.15 to about 0.75.

[0065] Aspect 2. The system according to Aspect 1, wherein the filling material includes a solid precursor material.

[0066] Aspect 3. The system according to Aspect 1 or Aspect 2, wherein the bulk density of the filling material is in the range of about 0.5 to about 2.

[0067] Aspect 4. The system according to any one of Aspects 1 to 3, wherein the vibration source includes two or more vibration devices.

[0068] Aspect 5. The system according to any one of Aspects 1 to 4, further including a funnel.

[0069] Aspect 6. The system according to Aspect 5, wherein the funnel is connected to the upper part of the container and is configured to guide the filling material into the container.

[0070] Aspect 7. The system according to any one of Aspects 1 to 6, wherein the container includes a filling port.

[0071] Aspect 8. The system according to Aspect 7, wherein the filling material enters the container through the filling port.

[0072] Aspect 9. A container comprising a sidewall and a bottom defining an internal volume, and a solid precursor material accommodated in the internal volume of the container, wherein the ratio of the solid precursor material includes that obtained by dividing the particle density of the solid precursor material by the bulk density of the solid precursor material after vibration, and the ratio of the solid precursor material is in the range of about 0.15 to about 0.75.

[0073] Aspect 10. The container according to Aspect 9, wherein the bulk density of the solid precursor material is in the range of about 0.5 to about 2.

[0074] Aspect 11. A method of filling the internal volume of a container with a filling material, the method including filling the internal volume of the container defined by the sidewall and the bottom of the container, vibrating the container to thereby increase the bulk density of the filling material, wherein the ratio of the filling material includes that obtained by dividing the particle density of the filling material by the bulk density of the filling material after vibration, and after increasing the bulk density of the filling material, the ratio of the filling material is in the range of about 0.15 to about 0.75.

[0075] Aspect 12. The method according to Aspect 11, wherein vibrating the container includes directly vibrating the body of the container.

[0076] Aspect 13. The method according to Aspect 11 or Aspect 12, wherein vibrating the container includes vibrating the container via one vibration device.

[0077] Aspect 14. The method according to any one of Aspects 11 to 13, wherein vibrating the container includes vibrating the container via two or more vibration devices.

[0078] Aspect 15. The method according to any one of Aspects 11 to 14, wherein vibrating the container includes continuously vibrating the container or applying vibration stepwise.

[0079] Aspect 16. The method according to any one of Aspects 11 to 15, wherein filling the internal volume of the container with the filling material includes introducing the filling material through a filling port of the container.

[0080] Aspect 17. The method according to aspect 16, wherein the diameter of the filling port ranges from about 0.25 inches to about 0.75 inches.

[0081] Aspect 18. The method according to any one of aspects 11 to 17, wherein vibrating the container reduces the porosity of the container containing the filling material.

[0082] Aspect 19. The method according to any one of aspects 11 to 18, wherein the filling material comprises a solid precursor material.

[0083] Aspect 20. The method according to any one of aspects 11 to 19, wherein the bulk density of the filling material ranges from about 0.5 to about 2.

[0084] In particular, it should be understood that changes may be made in detail, without departing from the scope of the present disclosure, with respect to the construction materials used and the shape, size, and arrangement of the components. The present specification and the described embodiments are examples, and the true scope and spirit of the present disclosure are indicated by the appended claims.

Claims

1. A container for containing a filling material, and a vibration source connected to the container, wherein the vibration source is configured to increase the bulk density of the filling material, the ratio of the filling material includes the particle density of the filling material divided by the bulk density of the filling material after vibration, and after increasing the bulk density of the filling material, the ratio of the filling material is in the range of about 0.15 to about 0.75 system.

2. The system according to claim 1, wherein the filling material includes a solid precursor material.

3. The system according to claim 1, wherein the bulk density of the filling material is in the range of about 0.5 to about 2.

4. The system according to claim 1, wherein the vibration source includes two or more vibration devices.

5. The system according to claim 1, further including a funnel.

6. The system according to claim 5, wherein the funnel is connected to the upper part of the container, and the funnel is configured to guide the filling material into the container.

7. The system according to claim 1, wherein the container includes a filling port.

8. The system according to claim 7, wherein the filling material enters the container through the filling port.

9. A side wall and a bottom defining an internal volume, and a solid precursor material contained in the internal volume of the container, wherein the ratio of the solid precursor material includes the particle density of the solid precursor material divided by the bulk density of the solid precursor material after vibration, and the ratio of the solid precursor material is in the range of about 0.15 to about 0.75 container.

10. The container according to claim 9, wherein the bulk density of the solid precursor material is in the range of about 0.5 to about 2.

11. Filling the internal volume of the container with a filling material, wherein the internal volume of the container is defined by the side wall and the bottom of the container, the filling, vibrating the container, thereby increasing the bulk density of the filling material, wherein the ratio of the filling material includes the particle density of the filling material divided by the bulk density of the filling material after vibration, and after increasing the bulk density of the filling material, the ratio of the filling material is in the range of about 0.15 to about 0.75 method.

12. The method according to claim 11, wherein vibrating the container includes directly vibrating the main body of the container.

13. The method according to claim 11, wherein vibrating the container includes vibrating the container through one vibration device.

14. The method according to claim 11, wherein vibrating the container includes vibrating the container through two or more vibration devices.

15. The method according to claim 11, wherein vibrating the container comprises vibrating the container continuously or applying vibrations stepwise. **Claim 16** The method according to claim 11, wherein filling the internal volume of the container with a filling material comprises introducing the filling material through a filling port of the container. **Claim 17** The method according to claim 16, wherein the diameter of the filling port is in the range of from about 0.25 inches to about 0.75 inches. **Claim 18** The method according to claim 11, wherein vibrating the container reduces the porosity of the container containing the filling material. **Claim 19** The method according to claim 11, wherein the filling material comprises a solid precursor material. **Claim 20** The method according to claim 11, wherein the bulk density of the filling material is in the range of from about 0.5 to about 2.

Images