阅读说明：本技术 调节器组合件及测试方法 (Regulator assembly and test method ) 是由 E·E·琼斯 S·A·乌茨 J·R·德斯普雷斯 于 2021-04-30 设计创作，主要内容包括：可使用经选择以具有约为从包含调节器组合件的流体存储及输送容器分配的选定流体的分子量的分子量的测试流体来测试调节器组合件。所述测试流体可为单种气体或混合物。所述测试流体可具有在从所述流体存储及输送容器分配的所述选定流体的所述分子量的80％到110％之间的分子量。当依此方式测试的调节器组合件在所述测试气体流启动时展示少于两个尖峰时,其可通过评估。可将这些调节器组合件安装到流体存储及输送容器中,尤其用于加压流体的存储及输送。(The regulator assembly may be tested using a test fluid selected to have a molecular weight that is about the molecular weight of the selected fluid dispensed from the fluid storage and delivery vessel that includes the regulator assembly. The test fluid may be a single gas or a mixture. The test fluid may have a molecular weight between 80% and 110% of the molecular weight of the selected fluid dispensed from the fluid storage and delivery container. A regulator assembly tested in this manner may be evaluated when it exhibits less than two spikes when the flow of test gas is initiated. These regulator assemblies may be installed into fluid storage and delivery vessels, particularly for the storage and delivery of pressurized fluids.)

1. A regulator assembly for a fluid supply container of a selected fluid, comprising:

a first regulator having an outlet pressure set to a predetermined set point; and

a second regulator configured to receive fluid from the first regulator,

wherein the predetermined set point is an outlet pressure that produces less than two spikes in flow through the second regulator when the regulator assembly operates with a test fluid having a molecular weight between 80% and 110% of the molecular weight of the selected fluid.

2. The regulator assembly of claim 1, wherein the test fluid is a mixture of two or more fluids and each of the two or more fluids is a gas.

3. The regulator assembly of claim 1, wherein the molecular weight of the test fluid is between 85% and 95% of the molecular weight of the selected fluid.

4. The regulator assembly of claim 1, wherein the selected fluid comprises CF₄、CO、BF₃、SiF₄、AsH₃、PH₃And GeF₄One or more of (a).

5. The regulator assembly of claim 4, wherein the selected fluid is further comprised of H₂A mixture of (a).

6. A fluid supply container comprising the regulator assembly of claim 1, wherein the fluid supply container is configured to store the selected fluid.

7. The fluid supply container of claim 6, wherein the selected fluid comprises CF₄、CO、BF₃、SiF₄、AsH₃、PH₃And GeF₄One or more of (a).

8. The fluid supply container of claim 7, wherein the selected fluid is further comprised of H₂A mixture of (a).

9. A method of testing a regulator, comprising:

introducing a test fluid into a plurality of test regulator assemblies, wherein:

the test fluid has a molecular weight between 80% and 110% of the molecular weight of the selected fluid supplied by the fluid supply package, and

each of the plurality of test regulator assemblies includes a first regulator and a second regulator, the first regulator of each of the plurality of test regulator assemblies having a predetermined outlet pressure;

monitoring a flow rate of the test fluid through the second regulator of each of the plurality of test regulator assemblies;

determining a number of spikes in the monitored flow through the second regulator of each of the plurality of test regulator assemblies; and

assembling a regulator assembly for the fluid supply package, the regulator assembly including the first regulator and the second regulator selected from one of the plurality of test regulator assemblies that exhibit less than two spikes in the observed flow rate.

10. The method of claim 9, wherein the first spike in observed flow is a pressure spike in the observed flow.

11. The method of claim 9, wherein the test fluid is a mixture of two or more fluids and each of the two or more fluids is a gas.

12. The method of claim 9, wherein the molecular weight of the test fluid is between 85% and 95% of the molecular weight of the selected fluid.

13. The method of claim 9, further comprising installing the supply package regulator assembly into the fluid supply package.

14. The method of claim 9, wherein the selected fluid comprises CF₄、CO、BF₃、SiF₄、AsH₃、PH₃And GeF₄One or more of (a).

15. The method of claim 14, wherein the selected fluid is further comprised of H₂A mixture of (a).

Technical Field

The present disclosure relates to methods for testing regulators used with fluid storage and delivery vessels, and more particularly, to testing regulators to identify regulators that provide acceptable spike performance.

Background

Pressure regulated fluid storage and delivery vessels may be used to supply fluids in industrial processes such as, for example, semiconductor manufacturing processes. Pressure regulation may be provided by a pressure regulator assembly that includes one or more pressure regulators.

Some pressure regulated fluid storage and delivery vessels may experience pressure fluctuations and instabilities when the dispensing of the fluid is initiated, particularly when the flow rate is initiated. Some industrial processes may be sensitive to such fluctuations and instabilities. As part of quality control screening for such products, pressure regulators for these fluid storage and delivery vessels can be tested to identify and reject regulator assemblies that provide spikes when flow is initiated at a particular pressure. Typically, a light inert gas is used as the test fluid for testing the regulator assembly, with the gas often being selected based on the cost and/or disposal characteristics of the fluid. When manufacturing pressure regulators, the rejection rate of the test significantly affects throughput, and improper rejection of components can result in significant waste and loss of pressure regulator production.

Disclosure of Invention

The present disclosure relates to methods for testing regulators used with fluid storage and delivery vessels, and more particularly, to testing regulators to identify regulators that provide acceptable spike performance.

Testing of a regulator assembly for a fluid storage and delivery vessel may be performed using a molecular weight that is closer to the molecular weight of the fluid dispensed by the regulator. This may provide a more accurate assessment of flow through the regular assembly. The improved evaluation increases the throughput rate of the test while continuing to provide adequate anti-spike protection for the flow through the regulator assembly. Reducing the false alarm rate of rejecting regulator assemblies can save costs and reduce waste as rejected assemblies are discarded or returned.

According to various embodiments of the present disclosure, some or all of the regulator assemblies assembled and installed into the fluid storage and/or delivery vessel may be tested to provide a quality assessment. According to various embodiments of the present disclosure, testing may alternatively be conducted to set design parameters, for example, to improve the selection of set design values, such as set points for outlet pressure of a regulator assembly.

In an embodiment, a method of testing a regulator for a fluid supply package includes introducing a test fluid into a plurality of separate test regulator assemblies. The test fluid has a molecular weight between 80% and 110% of the molecular weight of the selected fluid to be supplied by the fluid supply package. Each of the plurality of test regulator assemblies includes a first regulator and a second regulator, the first regulator of each of the plurality of test regulator assemblies having a set outlet pressure. The method further includes observing flow through the second regulator of each of the plurality of test regulator assemblies. The method further includes determining a number of spikes in the observed flow through the second regulator of each of the plurality of test regulator assemblies. The method also includes assembling a supply package regulator assembly of the fluid supply package, the supply package regulator assembly including the first regulator and the second regulator of one of the plurality of test regulator assemblies that exhibits less than two spikes in the observed flow.

In an embodiment, the first spike in the observed flow is a pressure spike in the observed flow.

In an embodiment, the test fluid is a mixture of two or more fluids, and each of the two or more fluids is a gas.

In embodiments, the molecular weight of the test fluid is between 85% and 95% of the molecular weight of the selected fluid.

In an embodiment, the method further includes installing the supply package regulator assembly into the fluid supply package.

In an embodiment, the selected fluid comprises CF₄、CO、BF₃、SiF₄、AsH₃、PH₃And GeF₄One or more of (a). In embodiments, the selected fluid is a fluid further comprising H₂A mixture of (a).

In an embodiment, a regulator assembly for a fluid supply container of a selected fluid includes: a first regulator having an outlet pressure set to a predetermined set point; and a second regulator configured to receive fluid from the first regulator. The predetermined set point is an outlet pressure that produces less than two spikes in flow through the second regulator when the regulator assembly operates with a test fluid having a molecular weight between 80% and 110% of the molecular weight of the selected fluid.

In an embodiment, the test fluid is a mixture of two or more fluids, and each of the two or more fluids is a gas.

In embodiments, the molecular weight of the test fluid is between 85% and 95% of the molecular weight of the selected fluid.

In an embodiment, the selected fluid comprises CF₄、CO、BF₃、SiF₄、AsH₃、PH₃And GeF₄One or more of (a). In embodiments, the selected fluid is a fluid further comprising H₂A mixture of (a).

In an embodiment, a fluid supply vessel includes a regulator assembly including: a first regulator having an outlet pressure set to a predetermined set point; and a second regulator configured to receive fluid from the first regulator, wherein the predetermined set point is an outlet pressure that produces less than two spikes in flow through the second regulator when the regulator assembly operates using a test fluid having a molecular weight between 80% and 110% of the molecular weight of the selected fluid. The fluid supply container is configured to store the selected fluid.

In an embodiment, the selected fluid comprises CF₄、CO、BF₃、SiF₄、AsH₃、PH₃And GeF₄One or more of (a). In embodiments, the selected fluid is a fluid further comprising H₂A mixture of (a).

Drawings

The disclosure may be more completely understood in view of the following description of various illustrative embodiments in connection with the accompanying drawings.

Fig. 1 shows a fluid storage and transport container according to an embodiment.

FIG. 2 shows a regulator assembly for a fluid storage and transport vessel, according to an embodiment.

FIG. 3 shows a flow chart of a method for testing a regulator assembly of a fluid storage and delivery vessel.

FIG. 4A shows a response of a regulator assembly to spike-free flow under test, according to an embodiment.

FIG. 4B shows a response of a regulator assembly to a flow including a spike when tested, according to an embodiment.

FIG. 5 shows a series of test results using the same regulator assembly and different test fluids.

While the disclosure is susceptible to various modifications and alternative forms, specific embodiments thereof have been shown by way of example in the drawings and will be described in detail. It should be understood, however, that there is no intention to limit aspects of the disclosure to the specific illustrative embodiments described. On the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the disclosure.

Detailed Description

The present disclosure relates to methods for testing regulators used with fluid storage and delivery vessels, and more particularly, to testing regulators to identify regulators that provide acceptable spike performance.

As used herein, "fluid" refers to one or more gases, one or more liquids, or a combination thereof.

Fig. 1 shows a fluid storage and transport container according to an embodiment. The fluid storage and delivery container 100 includes a container body 102 having an aperture 104. A regulator assembly 106 may be included in the bore 104 to control flow to and from the fluid storage and transport vessel 100. The regulator assembly 106 includes an inlet 108 (which may include a filter 110), a first regulator 112 that receives fluid from the inlet 108, a second regulator 114 that receives fluid from the first regulator 112, and a distributor 116 that receives fluid from the second regulator 114.

The fluid storage and delivery vessel 100 is a container for storing a fluid. The fluid is typically delivered in gaseous form. The fluid may be delivered by the fluid storage and delivery vessel 100 at a pressure below atmospheric pressure. The fluid may be stored in the fluid storage and delivery vessel 100 under pressure, such as at a pressure greater than atmospheric pressure. In an embodiment, the fluid storage and delivery container may be a vacuum actuated cylinder from Entegris, Inc(VAC) packaging. The fluid may be a fluid used in industrial processes such as semiconductor manufacturing, display assembly manufacturing, solar panel manufacturing, or the like. As a non-limiting example, the pressurized fluid may comprise AsH₃、AsF₃、AsF₅、PH₃、NF₃、PF₃、PF₅、BF₃、BCl₃、B₂H₆、Si₂H₆、Si₃H₈、SiH₄、C₃H₁₀Si、Si(CH₃)₄Halosilanes such as, for example, SiF₄) Halodisilanes such as, for example, Si₂F₆) Chlorosilanes (e.g. SiCl)₄)、GeH₄、GeF₄、H₂Se、H₂Te、SbH₃、CH₄、CF₄、CHF₃、CH₂F₂、CH₃F、CO、CO₂、COF₂、HS、H₂、HF、B₂F₄、HCl、Cl₂Fluorinated hydrocarbons, N₂、O₂、F₂He, Xe, Ar, Kr, organometallic gaseous reagents, mixtures of two or more of the foregoing, one or more of the foregoing with H₂Or any other suitable mixture of components and/or isotopically enriched variants of the foregoing. The fluid contained therein may be pressurized to any pressure suitable for the fluid being stored. In embodiments, within the fluid storage and delivery vessel 100The storage pressure may range from 200psig to 1550 psia. In an embodiment, the fluid storage and delivery vessel 100 may be configured to have a nominal storage pressure service pressure of up to 2265 psia.

The container body 102 can define an interior space for containing a fluid. The container body 102 may be made of any material suitable for a container. Suitable materials are capable of containing pressurized fluids without deformation. By way of non-limiting example, suitable materials may include one or more metals, gas impermeable polymers, fiber resin composites, combinations thereof, or the like. The container body 102 can include a sidewall 118 and a bottom 120 forming a generally cylindrical shape, with a neck 122 extending from the sidewall 118 toward an end 124. The end 124 can be opposite the bottom 120 of the container body 102.

The aperture 104 is an opening of the container body 102 located at the end 124. The regulator assembly 106 may pass through the aperture 104. The regulator assembly 106 can be sealed to the container body 102 in any suitable leak-proof manner such that the regulator assembly 106 controls the flow of fluid into and out of the container body 102 through the aperture 104. The regulator assembly 106 includes an inlet 108, a first regulator 112, a second regulator 114, and a distributor 116.

The inlet 108 is an opening that allows fluid within the container body 102 to pass into the regulator assembly 106. The inlet 108 may be connected to an inlet of a first regulator 112. Optionally, a filter 110 surrounding the inlet 108, covering the inlet 108, or within the inlet 108 may be included upstream of the first regulator 112 with respect to fluid passing into the regulator assembly 106 from the interior of the vessel body 102 and through the regulator assembly 106. The filter 110 is configured to ensure the purity of the gas and/or prevent particulate matter from entering the regulator assembly 106. The filter 110 may be any filter material suitable for use with the fluid contained within the fluid storage and delivery container 100. The filter 110 may be, for example, nickel, stainless steel, or polytetrafluoroethylene.

The first regulator 112 is a pressure regulator positioned between the inlet 108 and the second regulator 114 with respect to fluid flow through the regulator assembly 106. The first regulator 112 is a pressure regulator of the fluid. The first regulator 112 can reduce the pressure of the fluid from an inlet pressure at or near the pressure of the fluid within the vessel body 102 to a relatively lower intermediate pressure provided at the outlet of the first regulator 112. The first regulator 112 may be any suitable type of fluid pressure regulator capable of receiving fluid at an inlet pressure and providing it at a relatively lower outlet pressure. In an embodiment, the first regulator 112 may be configured to receive the fluid at an inlet pressure corresponding to the storage pressure of the fluid storage and delivery vessel 100, such as in a range between 200psig to 1550 psia. In an embodiment, the outlet pressure of the first regulator 112 may be determined based on testing according to the method shown in fig. 3 and described below. In an embodiment, the outlet pressure of the first regulator may be about 15 to 35 psig. In an embodiment, the outlet pressure of the first regulator 112 may be about 20 to 30 psig. In an embodiment, the outlet pressure of the first regulator is about 25 psig. Outlet pressures of the first regulator 112 within these ranges may reduce observed spike behavior observed from the outlet of the second regulator 114.

The second regulator 114 is a second pressure regulator of fluid configured to receive fluid from the first regulator 112 at substantially the outlet pressure of the first regulator 112 and to provide fluid at the outlet at a relatively lower pressure. The second regulator may be any pressure regulator adapted to receive fluid at the outlet pressure of the first regulator 112 and further reduce the pressure. The outlet pressure supplied by the second regulator 114 may be selected based on the application in which the fluid storage and delivery vessel 100 is used. In an embodiment, the outlet pressure supplied by the second regulator 114 may be a sub-atmospheric pressure. In an embodiment, the outlet pressure supplied by the second regulator 114 may range from 350 torr to 650 torr.

The first and second regulators 112, 114 may be first and second regulators, respectively, that pass a testing process (such as the testing process shown in fig. 3 and described below) before or after assembling them to the regulator assembly 106.

The pressure regulators that may be used as the first and second regulators 112, 114 may be, for example, regulators that use poppet valves to control flow from an inlet to an outlet of the pressure regulator. An example embodiment of such a regulator includes a main central housing in communication with inlet and outlet passages. A poppet valve is included in the inlet passage and engages a valve seat of the inlet passage to close the inlet passage to fluid flow. The poppet valve is coupled with a valve stem, which in turn is connected to a pressure sensing assembly in the interior volume of the pressure regulator. The pressure sensing assembly includes a plurality of diaphragms defining a bellows structure. The pressure sensing assembly is responsive to a pressure level in an outlet passage of the regulator such that a pressure in the outlet passage below a predetermined set point pressure will cause the plurality of diaphragms to move and cause the pressure sensing assembly and a poppet valve stem coupled thereto to correspondingly translate such that the poppet valve disengages its valve seat to allow fluid flow through the inlet passage and the central chamber of the regulator to the outlet passage to flow fluid out of a drain of the outlet passage. When the fluid pressure in the outlet passage exceeds the set point pressure of the regulator, the pressure sensing assembly will responsively translate the poppet valve stem and associated poppet valve such that the poppet valve engages the valve seat of the inlet passage to close the passage to the fluid flow therethrough.

The distributor 116 may include, for example, a valve 126 and a discharge port 128. Valve 126 controls flow through the regulator assembly to block or permit flow from the second regulator 114 toward the exhaust port 128. The vent 128 is an opening where fluid may exit the regulator assembly 106 to the exterior of the fluid storage and delivery vessel 100 when the valve 126 is in an open position that allows at least some flow therethrough. The fluid storage and delivery vessel 100 may further include attachment or retention features such that the vent 128 may be attached to provide fluid to, for example, an industrial tool, such as a tool for semiconductor processing, display manufacturing, solar panel manufacturing, or the like.

Fig. 2 shows a regulator assembly 200 for a fluid storage and transport vessel, according to an embodiment. The regulator assembly 200 includes an inlet 202 covered by a filter 204. The regulator assembly 200 further includes a first regulator 206 configured to receive fluid from the inlet 202, a second regulator 208 configured to receive fluid from an outlet of the first regulator 206, and a distributor 210 configured to receive fluid from an outlet of the second regulator 208.

The regulator assembly 200 may be assembled as a component for subsequent installation into or use with a container, such as by being placed into a bore of a container (e.g., bore 104 of container 100) and sealed such that fluid entering or exiting the container must pass through the regulator assembly 200.

In an embodiment, the regulator assembly 200 may be positioned in the vessel such that any one or more of the inlet 202, the first regulator 206, and the second regulator 208 are positioned within the interior space, and the remaining one or more of the first regulator 206, the second regulator 208, and the distributor 210 are positioned outside of the interior space defined by the vessel. Any such configuration may be used as long as the inlet 202 is positioned within the container and the dispenser 210 is outside the container. In embodiments, one or more of the first and second regulators 206, 208 may be positioned within the body of the container, within the neck of the container, and/or in the body of a valve that controls flow from the container.

The inlet 202 allows fluid to enter the regulator assembly 200 such that the fluid may pass through the regulator assembly 200. The inlet 200 may be a bore connected to a fluid line extending to the first regulator 206. The filter 204 may be positioned around the inlet 202, above or within the inlet 202, or along a fluid line from the inlet 202 to the first regulator 206. The filter 204 may be any filter suitable for use with a fluid that will flow through the regulator assembly 200.

The first regulator 206 is a fluid pressure regulator configured to reduce fluid from a relatively higher pressure at or about the pressure of the fluid received at the inlet 202 and provide fluid at a relatively lower outlet pressure. The outlet of the first regulator 206 may be provided to the second regulator 208, such as by a fluid line providing fluid communication from the outlet of the first regulator 206 to the inlet of the second regulator 208. In an embodiment, the first regulator is configured to accept fluid at a pressure selected based on the pressure of the fluid within the vessel in which the regulator assembly 200 is to be installed. In an embodiment, the outlet pressure of the first regulator 206 may be determined based on testing according to the method shown in fig. 3 and described below. In an embodiment, the outlet pressure of the first regulator 206 may be about 15 to 35 psig. In an embodiment, the outlet pressure of the first regulator 206 may be about 20 to 30 psig. In an embodiment, the outlet pressure of the first regulator is about 25 psig. Outlet pressures of the first regulator 206 within these ranges may reduce observed spike behavior observed from the outlet of the second regulator 208.

The second regulator 208 is a pressure regulator configured to receive fluid at or near the outlet pressure of the first regulator 206 and further reduce the pressure to a value suitable for delivery of the fluid, such as through the dispenser 210. The second regulator 208 may be any suitable fluid pressure regulator capable of performing this pressure reduction. In an embodiment, the outlet pressure supplied by the second regulator 208 may be a sub-atmospheric pressure. In an embodiment, the outlet pressure supplied by the second regulator 208 may range from 350 torr to 650 torr.

The first regulator 206 and the second regulator 208 may be first and second regulators, respectively, that pass a testing process (such as the testing process shown in fig. 3 and described below) before or after assembling them to the regulator assembly 200.

The pressure regulators that may be used as the first and second regulators 206, 208 may each be a regulator that controls flow from an inlet to an outlet of the pressure regulator, for example, using a poppet valve. An example embodiment of such a regulator includes a main central housing in communication with inlet and outlet passages. A poppet valve is included in the inlet passage and engages a valve seat of the inlet passage to close the inlet passage to fluid flow. The poppet valve is coupled with a valve stem, which in turn is connected to a pressure sensing assembly in the interior volume of the pressure regulator. The pressure sensing assembly includes a plurality of diaphragms defining a bellows structure. The pressure sensing assembly is responsive to a pressure level in an outlet passage of the regulator such that a pressure in the outlet passage below a predetermined set point pressure will cause the plurality of diaphragms to move and cause the pressure sensing assembly and a poppet valve stem coupled thereto to correspondingly translate such that the poppet valve disengages its valve seat to allow fluid flow through the inlet passage and the central chamber of the regulator to the outlet passage to flow fluid out of a drain of the outlet passage. When the fluid pressure in the outlet passage exceeds the set point pressure of the regulator, the pressure sensing assembly will responsively translate the poppet valve stem and associated poppet valve such that the poppet valve engages the valve seat of the inlet passage to close the passage to the fluid flow therethrough.

The distributor 210 allows for the controlled discharge of fluid received at the inlet 202 and passing through the regulator assembly 200. The distributor 210 may include a valve 212 that controls the flow from the outlet of the second regulator 208 to a discharge port 214. The drain 214 is an opening that allows fluid provided at the inlet 202 to exit the regulator assembly 200. The regulator assembly 200 may further include an attachment or retention feature such that the vent 214 may be attached to provide fluid to, for example, an industrial tool, such as a tool for semiconductor processing, display manufacturing, solar panel manufacturing, or the like.

The regulator assembly according to embodiments may include an additional regulator upstream of the first regulator 206, further reducing the pressure before reaching the first regulator 206, the first regulator 206 then reducing the pressure to an output pressure suitable for suction by the second regulator 208, the second regulator 208 in turn supplying fluid at a suitable pressure for delivery from the vessel. Tests according to embodiments, such as the embodiments described below and shown in fig. 3, may be used to determine the inlet and outlet pressures of some or all of the upstream and first regulators, as described below.

FIG. 3 shows a flow chart of a method for testing a regulator assembly of a fluid storage and delivery vessel. In the method 300, test regulator assemblies are assembled 302, a test fluid is introduced 304 into each of the test regulator assemblies, the flow rate is observed 306, the number of spikes of the observed flow rate is determined 308, and the regulator assembly for use in the vessel is obtained 310.

The method 300 may be used, for example, as a quality control test of a regulator in preparation for use in a fluid storage and delivery container product. The method 300 may be used to test and compare different regulator and setting parameters to determine regulator settings for use in a regulator assembly.

The test conditioner assembly is assembled at 302. Assembling the test regulator at 302 includes placing the first regulator in fluid communication with a source of test fluid and placing the second regulator in fluid communication with an outlet of the first regulator. The first and second regulators of the test regulator assembly may be the first and second regulators 112 or 206 and 114 or 208, respectively, such as described above and shown in fig. 1 and 2. In the test regulator assembly, the first regulator is upstream of the second regulator with respect to the test fluid flow provided at 304, corresponding to the first regulator between the inlet and the second regulator in the regulator assembly (e.g., regulator assemblies 106 and 200 described above and shown in fig. 1 and 2). In an embodiment, each of the first and second regulators are in a test setup to assemble a test regulator assembly at 302. In an embodiment, the first and second regulators are assembled into a complete regulator assembly (such as the regulator assembly 106 or 200 described above and shown in fig. 1 and 2), and then the test regulator assembly is placed in fluid communication with a test fluid source to assemble the test regulator assembly at 302.

A test fluid is introduced into each of the test regulator assemblies at 304. The test fluid may be delivered at a predetermined pressure. The predetermined pressure may correspond to, for example, a maximum pressure at which the selected fluid is to be stored in a vessel that includes the regulator assembly. In an embodiment, the predetermined pressure may be higher than the maximum pressure at which the selected fluid will be stored, e.g. such that there is a safety margin for the test results. The predetermined pressure may be selected based on tests run for experimental purposes for regulator characteristic selection or regulator assembly quality control evaluation. In an embodiment, the predetermined pressure may range from about 100psia to 1500 psia. In an embodiment, the predetermined pressure during the quality control evaluation of the regulator assembly is about 155 psia. A predetermined pressure is provided when the flow of test fluid is initiated at 304. The predetermined pressure may be maintained throughout the process of providing the test fluid to the test regulator assembly.

It should be appreciated that the test results and spike performance are affected by the molecular weight of the fluid flowing through the regulator assembly as described below and shown in fig. 5. For a selected fluid to be stored and dispensed from a container that includes the regulator assembly, the test fluid may be selected to have a molecular weight that is between 80% and 110% of the molecular weight of the selected fluid. In an embodiment, the test fluid is selected to have a molecular weight between 85% to 95% of the molecular weight of the selected fluid. For a selected fluid comprising a single compound, the molecular weight may be determined by any suitable means, for example by standard calculations of molecular weight. For a selected fluid that is a mixture, the molecular weight can be determined by, for example: gravimetrically analyzing the weight of a known volume of each addition, calculating a weighted average of the components of the mixture, testing a sample of the mixture to estimate the molecular weight, using a predetermined value supplied by the supplier of the material, or any other such suitable method of obtaining a molecular weight value for the mixture. In embodiments, the test fluid may comprise a single compound, and the molecular weight of the test fluid may be determined by any suitable means, such as by standard calculations of molecular weight. In embodiments, the test fluid is a mixture formed to have a selected molecular weight, as determined by, for example, a weighted average of the components of the mixture, a gravimetric measurement (including measuring the weight of each component of the mixture as it is added to the test mixture), or any other such method, wherein the selected molecular weight is within a range for the selected fluid.

The selected fluid may be any suitable fluid of interest to be delivered using the fluid storage and delivery container. Non-limiting examples of selected fluids include AsH₃、AsF₃、AsF₅、PH₃、NF₃、PF₃、PF₅、BF₃、BCl₃、B₂H₆、Si₂H₆、Si₃H₈、SiH₄、C₃H₁₀Si、Si(CH₃)₄Halosilanes such as, for example, SiF₄) Halodisilanes such as, for example, Si₂F₆) Chlorosilanes (e.g. SiCl)₄)、GeH₄、GeF₄、H₂Se、H₂Te、SbH₃、CH₄、CF₄、CHF₃、CH₂F₂、CH₃F、CO、CO₂、COF₂、HS、H₂、HF、B₂F₄、HCl、Cl₂Fluorinated hydrocarbons, N₂、O₂、F₂、He、Xe, Ar, Kr, organometallic gaseous reagents, mixtures of two or more of the foregoing, one or more of the foregoing with H₂Or any other suitable mixture of components and/or isotopically enriched variants of the foregoing.

The test fluid may be any suitable fluid having a molecular weight capable of being supplied at pressure and passed through the test regulator assembly as described above. The test fluid may comprise a single selected compound or a mixture of compounds. In an embodiment, the test fluid consists of an inert gas. As non-limiting examples, the test fluid may comprise one or more of hydrogen, helium, argon, krypton, xenon, carbon tetrafluoride, or mixtures thereof. In an example embodiment, the test fluid may be an argon-xenon mixture.

The flow is observed at 306. The observed flow may be a flow at an outlet of a second regulator of the test regulator assembly. The observation of the flow may include measuring one or more of a pressure of the dispensed gas, a velocity of the flow, a volumetric flow rate of the flow, or any other suitable measurement reflecting an amount of the flow through the second regulator over time. The observation of the flow rate is performed over time and includes initiating a flow rate of the test fluid. The observation may be made using any sensor suitable for making measurements, positioned at the outlet of or downstream of the second regulator of the test regulator assembly.

The number of spikes in observed traffic is determined at 308. The spike may be determined by, for example, processing data obtained while observing the flow at 306 to determine the number of peaks occurring in the measurement. The peaks may be identified by any processing technique suitable for the data. Examples of a plurality of such peaks can be seen, for example, in fig. 4B and 5 and described below. The number of spikes of the observed flow determined at 308 may then be compared to a threshold for passing or rejecting the regulator of the test regulator assembly. The threshold may be any threshold of spike performance acceptable by the application of the regulator assembly in which the regulator assembly or fluid storage and delivery vessel will be used, and may vary with the application. In an embodiment, two or more spikes result in the regulator of the test regulator assembly being rejected. In an embodiment, less than two spikes cause the regulator of the test regulator assembly to pass through for use in the regulator assembly of the fluid storage and delivery vessel. In some embodiments, both spikes may also be considered acceptable and passed through for use. In an embodiment, multiple test regulator assemblies having different parameters (e.g., first regulator outlet pressure) may be prepared at 302 and supplied and observed flow rates at 304, 306, with the passing or failing of the test regulator being used to determine acceptable or preferred values for the parameter varying between the different test regulator assemblies.

A regulator assembly for use with the vessel is optionally available at 310. When the test regulator assembly passes after determining at 308 that the number of spikes is below the threshold, some or all of the components of the test regulator assembly may be used to obtain a regulator assembly for use with the container. In an embodiment, assembling the regulator assembly at 310 may include employing first and second regulators from the test regulator assembly assembled at 302 and providing a distributor connected to an inlet of the first regulator, a fluid line connecting an outlet of the first regulator to the second regulator, and an outlet connected to the second regulator to, for example, obtain the arrangement shown for the regulator assembly 106 or 200 described above and shown in fig. 1 and 2.

Optionally, the regulator assembly assembled at 310 may be further assembled into a fluid storage and delivery vessel at 312. The regulator assembly 310 can be installed into an aperture of a container, such as the aperture 104 of the container body 102 shown in fig. 1 and described above, with the regulator assembly sealed such that all fluid must travel through the regulator assembly to enter or exit the resulting container. The fluid storage and delivery vessel may then be used to store and deliver a pressurized fluid, such as any of the fluids listed above.

FIG. 4A shows an example response of a regulator assembly to spike-free traffic under test, according to an embodiment. As can be seen in fig. 4A, the pressure dropped to a minimum of 400 torr over time. Time T-0 is assigned to the occurrence of this minimum value. After the minimum pressure value is reached, the pressure smoothly recovers to slightly above 400 torr, with the pressure remaining as the test fluid continues to flow until T ═ 120 seconds, as indicated by the "SCCM" line. The example response shown in fig. 4A will provide a smooth, consistent pressure of fluid delivered from within a fluid storage and delivery vessel suitable for use with even sensitive industrial tools, such as tools for semiconductor, device, or solar panel manufacturing.

FIG. 4B shows a response of a regulator assembly to a flow including a spike when tested, according to an embodiment. In the results shown in fig. 4B, the pressure dropped to a minimum below 350 torr. For the purpose of the graph, the time T-0 is set as the point in time where the minimum pressure value is achieved. The pressure rose back almost immediately to 425 torr, then dropped sharply to 375 torr, then rose back almost immediately to about 425 torr again, and thereafter dropped gradually and smoothly to 400 torr until the test fluid supply ended, as shown by the SCCM line on the graph. The two upward spikes in pressure, along with the second dip, represent spike behavior that may be observed in some regulator assemblies. In some regulator assemblies, the spikes may be further repeated, providing continuous oscillation between relatively high and relatively low pressures. Some industrial tools, such as some tools used for semiconductor, display, or solar panel manufacturing, are unable to handle such inconsistencies in the pressure of the supplied fluid. Such inconsistencies may, for example, cause product loss, expensive down time of the process tool or flow interruptions through the manufacturing line, or other waste of components, time, and/or material. Thus, the spike behavior shown by multiple dips followed by bumps may not be suitable in fluid storage and delivery containers for such sensitive applications. Typically, a single spike is acceptable in many applications of fluid storage and delivery containers, while two or more such spikes would require rejection of the regulator assembly. However, it should be appreciated that the tolerance of the spike may vary from application to application, and acceptance or rejection of the regulator assembly may be appropriate or inappropriate based on the particular requirements of a particular application based on the spike behavior of the regulator assembly.

FIG. 5 shows a series of test results using the same regulator assembly and different test fluids. The result shown in fig. 5 is that in the trials obtained therefrom, the same regulator assembly with the same outlet pressure from the first regulator was used for each of the trials, with only the test fluid supplied being changed. In the first experiment shown in fig. 5, helium was used as the test fluid. In a second experiment, nitrogen was used as the test fluid. In a third experiment, argon was used as the test fluid. In a fourth experiment, an argon-xenon mixture was used as the test fluid. In a fifth experiment, xenon was used as the test fluid. As can be seen in the corresponding results, the test fluid with the relatively higher molecular weight resulted in fewer spikes and oscillations than the relatively lower molecular weight test fluid, even though the regulator assembly and outlet pressure were the same in all experiments. Thus, it should be appreciated that the spike and oscillation behavior observed in the flow rate varies with the molecular weight of the fluid passing through the regulator assembly, with fluids having lighter molecular weights resulting in increased spikes and oscillations over fluids having heavier molecular weights. Thus, testing using a test fluid having a molecular weight indicative of a selected fluid being conveyed through the regulator assembly may ensure a more accurate representation of the performance of the regulator assembly with which the selected fluid is used. Also, a test fluid having a relatively lower molecular weight than the selected fluid may provide a safety margin to the test, the test fluid being more susceptible to spikes and oscillations than would be experienced when used with the selected fluid.

The method comprises the following steps:

it is to be understood that any of aspects 1-7 may be combined with any of aspects 8-15.

Aspect 1. a method of testing a regulator for a fluid supply package, comprising:

introducing a test fluid into a plurality of individual test regulator assemblies, wherein:

the test fluid has a molecular weight between 80% and 110% of the molecular weight of the selected fluid supplied by the fluid supply package, and

each of the plurality of test regulator assemblies includes a first regulator and a second regulator, the first regulator of each of the plurality of test regulator assemblies having a set outlet pressure;

observing flow through the second regulator of each of the plurality of test regulator assemblies;

determining a number of spikes in the observed flow through the second regulator of each of the plurality of test regulator assemblies; and

assembling a supply package regulator assembly for the fluid supply package, the supply package regulator assembly including the first regulator and the second regulator of one of the plurality of test regulator assemblies exhibiting less than two spikes in the observed flow.

The method of aspect 1, wherein the first spike in the observed flow is a pressure spike in the observed flow.

Aspect 3. the method of any one of aspects 1-2, wherein the test fluid is a mixture of two or more fluids, and each of the two or more fluids is a gas.

Aspect 4. the method of any one of aspects 1-3, wherein the molecular weight of the test fluid is between 85% and 95% of the molecular weight of the selected fluid.

Aspect 5. the method of any of aspects 1-4, further comprising installing the supply package regulator assembly into the fluid supply package.

Aspect 6. the method of any of aspects 1-5, wherein the selected fluid comprises CF₄、CO、BF₃、SiF₄、AsH₃、PH₃And GeF₄One or more of (a).

Aspect 7 the method of aspect 6, wherein the selected fluid is further comprised of H₂A mixture of (a).

Aspect 8 a regulator assembly for a fluid supply vessel of a selected fluid, comprising:

a first regulator having an outlet pressure set to a predetermined set point; and

a second regulator configured to receive fluid from the first regulator,

wherein the predetermined set point is an outlet pressure that produces less than two spikes in flow through the second regulator when the regulator assembly operates with a test fluid having a molecular weight between 80% and 110% of the molecular weight of the selected fluid.

Aspect 9 the regulator assembly of aspect 8, wherein the test fluid is a mixture of two or more fluids, and each of the two or more fluids is a gas.

Aspect 10 the regulator assembly of any of aspects 8-9, wherein the molecular weight of the test fluid is between 85% to 95% of the molecular weight of the selected fluid.

Aspect 11 the regulator assembly of any of aspects 8-10, wherein the selected fluid includes CF₄、CO、BF₃、SiF₄、AsH₃、PH₃And GeF₄One or more of (a).

Aspect 12 the regulator assembly of aspect 11, wherein the selected fluid is further comprised of H₂A mixture of (a).

Aspect 13 a fluid supply container comprising the regulator assembly of any one of aspects 8-10, wherein the fluid supply container is configured to store the selected fluid.

Aspect 14 the fluid supply vessel of aspect 13, wherein the selected fluid comprises CF₄、CO、BF₃、SiF₄、AsH₃、PH₃And GeF₄One or more of (a).

Aspect 15 the fluid supply vessel of aspect 14, wherein the selected fluid further comprises H₂A mixture of (a).

While several illustrative embodiments of the present disclosure have been thus described, those skilled in the art will readily appreciate that other embodiments may be made and used within the scope of the appended claims. Numerous advantages of the disclosure covered by this document have been set forth in the foregoing description. However, it should be understood that this disclosure is, in many respects, only illustrative. Changes may be made in details, particularly in matters of shape, size, and arrangement of parts, without exceeding the scope of the disclosure. The scope of the present disclosure is, of course, defined in the language in which the appended claims are expressed.