JP5596804B2 - Splash guard for high flow vacuum bubbler containers - Google Patents

Description

  This patent application is filed with US patent application serial no. This is a continuation-in-part of 12 / 407,279.

  Electronic equipment manufacturers use chemical precursor containers. This container converts liquid chemicals into vaporized chemicals for supply to an electronics manufacturing reactor (ie, an apparatus for performing chemical vapor deposition “CVD”). CVD is a preferred technique for forming layers, films, and other deposits in the construction of electronic manufacturing such as, for example, integrated circuits or computer chips. For the efficiency of transporting and storing a certain amount of chemical precursor, a liquid or solid is preferred as a source. However, in the industry, it is desirable to actually supply the chemical precursor in the apparatus area in the form of a vaporized gas (ie, CVD). Alternatively, some manufacturing is done using direct liquid injection (“DLI”). However, even in that case, the liquid is vaporized in the apparatus after supply.

  When utilizing vaporized gas supply in CVD, the container typically has an inert carrier gas. The inert carrier gas is passed through the vessel or bubbled (ie, a bubbler) and carries the vaporized chemical precursor gas entrained in the inert carrier gas to the apparatus. The bubbler typically has a lower tube inlet at which the carrier gas is introduced into the container below the liquid chemical precursor level. Here, the carrier gas is bubbled through the liquid chemical precursor. At this time, as the carrier gas floats the liquid as bubbles, the chemical precursor is taken in, and then flows out of the container or bubbler by the outlet installed on the liquid surface of the chemical precursor.

  Even if the chemical precursor is a small droplet, it is not preferable that the chemical precursor flows out of the container through the outlet in the form of a liquid. A uniform vaporized gas is preferred as such bubbler supply. This avoids corrosion, uneven flow, and aerosol droplets that can accumulate in the outlet pipe and form particles during manufacturing and container shut-off, reducing the frequency of cleaning.

  Various forms of bubbler splash guards have been tried in the industry to address this challenge. These include, for example, US Patent Application No. 2008/0143002, US Patent No. 6,520,218, European Patent Application No. 1329540, US Patent Application No. 2004/0013577, European Patent Application No. 0420596, US Pat. 589,110, U.S. Pat. No. 7,077,388, U.S. Patent Application 2003/0042630, U.S. Pat. No. 5,776,255, and U.S. Pat. No. 4,450,118. Yes. Each of these attempts to provide a splash guard function did not satisfy the desired performance. However, the present invention has succeeded in providing a high level splash guard function while enabling a high flow rate of chemical precursor, a flow under a high vacuum, or a flow in a high differential pressure state as disclosed below. did. This will be described below.

  The present invention relates to a container having the following configuration. The container includes a dip tube inlet, at least one baffle disk, an annular deflection protrusion, a shoulder, and a level sensor. Here, the dip tube inlet terminates in the vicinity of the base portion of the container. The baffle disk is configured as a shallow cone that opens downward, is positioned between the outlet of the dip tube and the outlet of the container, and is narrow between the baffle disk and the inner surface of the side wall of the container It is configured to form an annular space. The deflection protrusion is provided in the vicinity of the baffle disk so as to protrude radially inward on the side wall. The baffle disk and deflection protrusion can minimize liquid droplets entering the outlet of the container. The shoulder portion has an annular end portion that protrudes inward in the radial direction and is spaced apart from the innermost end of the deflection projection in the axially lower side. The level sensor terminates near the base of the container, and the container can have a liquid level above the end of the level sensor.

  Preferably, the deflection protrusion has an innermost end located radially inward from the outermost end of at least one baffle disk.

  Preferably, the deflection protrusion has a shoulder portion below the innermost end of the deflection protrusion, and the shoulder portion is radially inward from the inner surface of the side wall of the container so as not to exceed the innermost end of the deflection protrusion. Protrusively.

  Preferably, the at least one baffle disk, the deflection projection and the shoulder are arranged on the top of the container.

  Preferably, the deflection protrusion is provided between the upper baffle disk and the lower baffle disk and spaced apart from the upper baffle disk and the lower baffle disk in the axial direction.

  Preferably, the deflection protrusion is provided to be separated from the two baffle disks in the axially lower side.

  Preferably, the inlet to the outlet of the container has a bent structure that can minimize liquid entering the outlet of the container.

  Preferably, the inlet leading to the outlet of the container has a T-shape that can minimize liquid entering the outlet of the container.

  Preferably, the container has a cylindrical shape.

  The present invention also relates to a cylindrical vaporized gas generating container. A vaporized gas generating container according to the present invention includes a dip tube inlet capable of supplying a carrier gas into the container, a baffle disk having a circular shape and recessed on the lower side, an annular deflecting protrusion, a shoulder, a level A sensor. Here, the baffle disk is positioned between the outlet end of the dip tube inlet and the outlet of the container, and a narrow annular shape is formed between the outermost peripheral edge of the baffle disk and the inner surface of the container side wall. Configured to form a space. The deflection protrusion is provided in the vicinity of the baffle disk so as to protrude radially inward on the side wall, and has an innermost end located radially inward from the outermost peripheral edge of the baffle disk, and vaporizes from the container. To supply the liquid as a gas, liquid droplets entering the outlet of the container can be minimized when the carrier gas is bubbled through the liquid contents of the container. The shoulder portion has an annular end portion that protrudes inward in the radial direction and is spaced apart from the innermost end of the deflection projection in the axially lower side. The level sensor terminates near the base of the container, and the container can have a liquid level above the end of the level sensor.

  The present invention also relates to a liquid supply container. The liquid supply container according to the present invention includes at least one baffle disk, an annular deflecting protrusion, a shoulder, and a level sensor. Here, the baffle disk is configured as a shallow cone that opens downward, and is positioned between the inlet end of the dip tube outlet and the inlet of the liquid supply container, and the baffle disk and the side wall of the container A narrow annular space is formed between the inner surface and the inner surface. The deflection protrusion is provided in the vicinity of the baffle disk so as to protrude radially inward on the side wall, and has an innermost end positioned radially inward from the outermost end of the baffle disk, and is a liquid supply container Liquid droplets entering the inlet can be minimized. The shoulder portion has an annular end portion that protrudes inward in the radial direction and is spaced apart from the innermost end of the deflection projection in the axially lower side. The level sensor terminates near the base of the container, and the container can have a liquid level above the end of the level sensor.

  The present invention also relates to a process for supplying a chemical precursor from a container. The process includes the steps of conveying a carrier gas through the dip tube of the vessel, taking a liquid chemical precursor from the vessel into the carrier gas, and between the outermost end of the baffle disk and the inner surface of the vessel sidewall. The step of transporting the chemical precursor and the transport gas in a narrow annular space so as to pass through the deflection projection provided to project radially inwardly on the narrow annular space side wall and at least one baffle disk. With.

1 is a schematic side view of a portion of an embodiment of the present invention. 1 is a schematic side partial cross-sectional view of an embodiment of the present invention. It is a schematic side fragmentary sectional view of the 2nd Embodiment of this invention. It is a schematic side fragmentary sectional view of the 3rd Embodiment of this invention. It is a schematic side fragmentary sectional view of the 4th Embodiment of this invention.

  The present invention is a vaporized gas generating bubbler vessel configured for operation in high vacuum or high flow conditions. This configuration prevents aerosol droplets from being scattered or transferred into the supply line outlet. Here, the scattering or transfer of aerosol droplets into the supply line outlet will result in an abnormal mass flow rate of the chemical.

  Semiconductor manufacturers are starting to use high-value chemicals. These chemicals are very difficult to transport for deposition on a wafer in a vacuum chamber or apparatus. The bubbler container of the present invention enables liquid chemicals to be supplied from the container as vaporized gas under high vacuum without causing aerosol droplets to scatter and form at the outlet of the container. Here, the scattering and formation of the aerosol droplets at the outlet of the container results in an abnormal mass supply rate of the chemical substance. The present invention has a low surface configuration, which makes it possible to reduce the constant saturation of the carrier gas containing the chemical vaporization gas to a very low level of residual chemicals. Nevertheless, the present invention prevents the scattering and formation of aerosol droplets at the outlet of the container, which results in an abnormal mass feed rate of the chemical, even when the level of chemical in the container is high. In the past, containers used for high vacuum or high flow operation had to be used with only a partial charge of the chemical (ie, 50% full). This has required semiconductor manufacturers to change containers more frequently, increasing the cost of chemicals due to increased container processing costs. The present invention allows containers to be used from the highest level liquid chemicals to very low level liquid chemicals, reducing the downtime of semiconductor devices. Also, generation of particulates that can be caused by the decomposition of fuming droplets that accumulate in the outlet and all supply pipes leading to the processing chamber or equipment, as it is effective to limit fuming chemical particles at the outlet Can be reduced. In this description, it is preferable to provide a cylindrical container having a cylinder axis on a vertical plane. Thus, the description of shaft and diameter relates to the shape and orientation of this type of container.

  The present invention uses an annular deflection protrusion provided on the inner surface of the side wall of the container and protruding radially inward. In addition, the present invention uses one or more baffle disks disposed on the top of the container along with the deflection protrusions. With this configuration, the carrier gas in which the chemical precursor is taken in is flowed in a narrow annular space to the radially innermost end of the deflection protrusion and the outer part of the baffle disk, thereby indirectly at the outlet of the container. Transport. The narrow annular space is a space formed between the inner diameter of the inner surface of the side wall of the bubbler and the outermost diameter (or the end of the circumference or outer circumference) of the baffle disk. This configuration will be described with reference to a preferred embodiment of the present invention.

  FIG. 1 shows a bubbler container 10 of the present invention. The bubbler container 10 includes a cylindrical bubbler sidewall 12 having a dip tube inlet 14. The dip tube inlet 14 terminates at an inlet end located below the liquid level of the liquid chemical precursor. The liquid level of the liquid chemical precursor is indicated by a line 15 and is located above the base portion 13 of the container.

  The splash guard includes (1) a baffle disk 24 and (2) an annular deflection protrusion 22 that protrudes radially inward on the inner surface 23 of the side wall 12. Here, the baffle disk 24 preferably has a circular outermost peripheral edge shape, and is recessed on the lower side, for example, a shallow cone that opens downward. The baffle disk 24 and the deflection protrusion 22 cooperate to form a complex flow path for the chemical precursor that flows out of the container 10. The baffle disk 24 is recessed on the lower side to further prevent the chemical precursor from flowing directly to the outlet 16 and to agglomerate to return the coalesced droplets to the stored chemical precursor by dropping them back. Collect the chemical precursors (not shown). The baffle disk 24 has a diameter slightly smaller than the inner diameter of the cylindrical inner surface 23 of the side wall 12 of the container 10. The space between the outermost peripheral edge of the baffle disk 24 and the inner surface 23 of the side wall 12 of the container 10 is sufficient to allow gas to pass through the space with a minimal pressure drop. However, the space is sufficient to minimize the passage of liquid that can be released from the liquid content of the bubbler under high flow rates of carrier gas through the dip tube or under large pressure fluctuations. ,narrow. The container 10 comprises an upper part 17 and a lower part 11 and an exemplary liquid level 15. The liquid level 15 varies based on the degree of filling and the supply period, but is typically below the deflection protrusion 22 and baffle disk 24 and at the end of the inlet 14 and level sensor 28 (27a, respectively). And 27b).

  FIG. 2 separately shows the internal structure of the container according to this embodiment in which the dip tube 14 is omitted. A level sensor 28 is shown in the middle of the container and monitors the level of liquid chemicals. The level sensor 28 terminates in the vicinity of the base portion 13 of the container 10. Valve 30 controls the introduction of push or carrier gas that is routed through inlet 14 to the bottom of the vessel. In the lower part of the container, the carrier gas is bubbled through the liquid chemical substance, and the vaporized chemical substance is taken into the bubbles of the carrier gas. The liquid chemical substance is vigorously stirred by the bubbling action of the carrier gas when it flows out from the lower end of the inlet dip tube 14. Liquid chemicals are also vigorously (rigidly) stirred by the high vacuum at the outlet 16 when the valve 26 is open. Either of these causes the liquid chemical to bubble or scatter toward the outlet 16. A radially inwardly projecting annular deflection projection 22 associated with the side wall 12 of the container or bubbler 10 deflects any bubbled or splashed liquid chemical from near the outermost end of the baffle disk 24. It works like that. As a result, the deflecting projection 22 protects the inlet end 32 of the outlet 16 because the liquid chemical substance is sucked into the inlet end 32 instead of the vaporized gas of the chemical substance taken into the carrier gas. The baffle disk 24 and the deflection protrusion 22 form a complex flow path 38 for the chemical precursor that flows out of the container 10.

  In a preferred embodiment, the deflection projections 22 are formed from a portion of the side wall 12 during milling of the container or bubbler 10 from a solid piece of stainless steel material. The deflection protrusion 22 may have a conical cross-sectional structure and terminates at its innermost end 34. The innermost end 34 of the deflection protrusion 22 is located on the radially inner side of the outermost end 36 of the baffle disk 24. The deflection protrusion 22 may be an annular rim formed over the entire periphery of the inner surface 23 of the side wall 12. The combination of the baffle disk 24 and the deflection projection 22 forms a complex flow path 38 for the carrier gas and the vaporized gas of the incorporated chemical. Such a channel is very difficult for liquid phase chemicals to flow through.

  Preferably, the baffle disk 24 is axially above the deflection projection 22 so as to form a very narrow flow path (which is sufficient for vaporized gas to pass but difficult for liquid to pass). Spaced apart (ie, close to each other). Alternatively, the baffle disk 24 may be provided to be separated from the deflection protrusion 22 in the axially lower side. Further alternatively, the present invention contemplates multiple baffle disks. For example, as shown in FIG. 3, the baffle disk 24 is provided apart from the deflection protrusion 22 in the axial direction, and the baffle disk 24 a is provided separately from the deflection protrusion 22 in the axially lower side. Alternatively, as shown in FIG. 5, the two baffle disks 24 and 24 b are provided apart from the deflection protrusion 22 in the axial direction. Alternatively, as shown in FIG. 4, the two baffle disks 24, 24 d are provided to be separated from the deflection protrusion 22 in the axially lower side. Alternatively, the deflection protrusions are provided separately on the upper side and the lower side in the axial direction of each baffle disk. Alternatively, a plurality of baffle disks and deflection protrusions are provided. Preferably, all baffle disks and deflection protrusions are in close proximity to each other as defined above.

  The experiment showed that: That is, the bubbles move upward on the side wall 12 of the container or bubbler 10 from the end of the inlet dip tube 14, at this time, near the inner surface 23 of the side wall 12 of the container 10. Maximum flow is generated. Therefore, in one embodiment, the deflection protrusion 22 has a shoulder portion 21, and the shoulder portion 21 is provided radially inwardly spaced from the innermost end 34 of the deflection protrusion 22. It is formed as an annular end projecting into The deflection protrusion 22 and the shoulder 21 are configured as follows. That is, the deflection protrusion 22 protrudes radially inward so as to exceed the protrusion of the shoulder portion 21 inward in the radial direction. This shoulder may be integral with the entire portion of the deflection projection 22 and may be machined from a single piece of stainless steel (or other material) simultaneously with the deflection projection. The shoulder 21 performs two functions. The shoulder 21 forms a steep angle with respect to the inner surface 23, thereby changing the direction of the flow of the liquid rising on the inner surface to the inside of the container 10, and each of the baffle disk 24 and the deflection protrusion 22. The liquid flow is directed away from the complex flow path 38 formed by the ends of the liquid crystal. Also, any liquid collected on the deflection protrusion 22 will be discharged to the shoulder 21 and then dropped back into the liquid chemical stored in the lower part of the container or bubbler 10.

  The baffle disk 24 and the deflection protrusion 22 are preferably shown as being located in the upper region 17 of the container. However, as will be appreciated by those skilled in the art, the baffle disk 24 and deflecting protrusion 22 are within the standard upper limit of chemicals filled in the container, headspace, or position above the freeboard (at least above level 15). However, it will be understood that other locations are also contemplated.

  In the present embodiment, the deflection protrusion 22 and the shoulder portion 21 are integrated with each other and are provided integrally with the side wall. However, the deflection projections 22 and shoulders 21 may be separate members attached to the sidewalls by, for example, welding, friction fitting, or mechanical fixation with bolts, screws, and similar fasteners. Even if it is an individual member, the deflection protrusion 22 and the shoulder portion 21 may be integrated with each other or may be members separated from each other.

  Deflection protrusion 22, shoulder 21, and baffle disk 24 cooperate to form a complex flow path 38 for chemicals fed through outlet 16. In one example, under high vacuum or high flow rate, the liquid tends to bubble above the liquid level 15 and into the headspace of the upper region 17 of the container 10. The complex flow path 38 formed by the deflection protrusion 22, the shoulder 21 and the baffle disk 24 substantially prevents such bubbles from reaching the outlet 16.

  Although stainless steel has been described with respect to certain embodiments, the present invention may be used with different metals, glasses, and resins, including soft iron, monel alloys, nickel alloys, and similar manufacturing materials known to those skilled in the art. Good.

  The present invention can satisfactorily minimize the droplets being taken into the outlet and downstream pipe of the container connected to the CVD apparatus of the electronic device manufacturing system. By using a single baffle disk or a plurality of baffle disks in combination with deflecting protrusions, it is possible to minimize the entrainment of droplets at the bubbler outlet 16 as desired.

  The baffle disk was shown as a circular disk with a recess and slightly smaller than the inner diameter of the cylindrical container or bubbler sidewall. However, it will be understood that any baffle of any shape that simply provides a narrow annular space within the sidewall of the container is within the scope of the present invention. Similarly, any form of deflection projection having an end that projects smoothly radially inward or that includes a portion that deviates somewhat from a smooth annular curve is also contemplated as part of the present invention. .

  Although it is preferred to use stainless steel, any inert material that is in hard form may be used for the splash guard. Resins, metal alloys, powder metals, fabrics, fibers, and ceramics are all conceivable.

  The container 10 may also be used in the direction of product flow in the opposite direction. Here, the outlet 16 functions as a pressurized gas inlet for forming a pressure head on the liquid stored in the container 10. Contrary to the supply of the vaporized gas described above, the supply liquid is transported as a liquid phase from the container to the outside of the liquid supply dip tube 14 using the pressurized gas.

Claims (11)

A container for vaporizing and supplying chemical substances,
A dip tube inlet,
At least one baffle disk;
An annular deflection projection;
Shoulder and
And the level sensor, the Bei example,
The dip tube inlet terminates near the base of the container,
The baffle disk is
Constructed as a shallow cone opening towards the bottom,
Positioned between the outlet of the dip tube and the outlet of the container; and
A narrow annular space is formed between the baffle disk and the inner surface of the side wall of the container;
The deflection protrusion is provided in the vicinity of the baffle disk so as to protrude radially inward on the side wall,
The baffle disk and the deflecting projection can minimize liquid droplets entering the outlet of the container;
The shoulder portion has an annular end portion that protrudes inward in the radial direction, spaced apart from the innermost end of the deflection protrusion in the axially lower side,
The level sensor terminates in the vicinity of the base of the container, and the container may have a liquid level above the end of the level sensor.   The container according to claim 1, wherein the deflection protrusion has an innermost end located radially inward from an outermost end of the at least one baffle disk. The deflection protrusion has a shoulder on the lower side of the innermost end of the deflection protrusion,
The container according to claim 2, wherein the shoulder projects radially inward from the inner surface of the side wall of the container so as not to exceed the innermost end of the deflection protrusion.   The container of claim 3, wherein the at least one baffle disk, the deflection protrusion, and the shoulder are disposed on top of the container.   2. The container according to claim 1, wherein the deflecting protrusion is provided between the upper baffle disk and the lower baffle disk and is axially separated from the upper baffle disk and the lower baffle disk.   The container according to claim 1, wherein the deflecting protrusion is provided to be separated from two baffle disks in the axially lower side.   The container according to claim 1, wherein the inlet leading to the outlet of the container has a bent structure capable of minimizing liquid entering the outlet of the container.   The container according to claim 1, wherein the inlet leading to the outlet of the container has a T-shaped structure capable of minimizing liquid entering the outlet of the container.   The container according to claim 1, wherein the container has a cylindrical shape. A cylindrical vaporized gas generation container for vaporizing and supplying chemical substances ,
A dip tube inlet capable of supplying carrier gas into the container;
A baffle disk having a circular shape and recessed on the lower side;
An annular deflection projection;
Shoulder and
A level sensor,
The baffle disk is
Positioned between the outlet end of the dip tube inlet and the outlet of the container; and
A narrow annular space is formed between the outermost peripheral edge of the baffle disk and the inner surface of the side wall of the container,
The deflection protrusion is
On the side wall, provided in the vicinity of the baffle disk so as to protrude radially inward,
The innermost end located radially inward from the outermost peripheral edge of the baffle disk;
In order to supply liquid as vaporized gas from the container, liquid droplets entering the outlet of the container can be minimized when the carrier gas is bubbled through the liquid content of the container. ,
The shoulder portion has an annular end portion that protrudes inward in the radial direction, spaced apart from the innermost end of the deflection protrusion in the axially lower side,
The level sensor is terminated in the vicinity of the base of the container, and the container can have a liquid level above the end of the level sensor. A liquid supply container for vaporizing and supplying chemical substances,
At least one baffle disk;
An annular deflection projection;
Shoulder and
And the level sensor, the Bei example,
The baffle disk is
Constructed as a shallow cone opening towards the bottom,
Positioned between the inlet end of the dip tube outlet and the inlet of the liquid supply container; and
A narrow annular space is formed between the baffle disk and the inner surface of the side wall of the container;
The deflection protrusion is
On the side wall, provided in the vicinity of the baffle disk so as to protrude radially inward,
An innermost end located radially inward from the outermost end of the baffle disk;
Liquid droplets entering the inlet to the liquid supply container can be minimized,
The shoulder portion has an annular end portion that protrudes inward in the radial direction, spaced apart from the innermost end of the deflection protrusion in the axially lower side,
The level sensor is terminated near the base of the container, and the container can have a liquid level above the end of the level sensor.

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