Systems and methods for sample testing for battery- related materials
Patent Information
- Application Number
- PCT/US2026/021238
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2025-03-28
- Filing Date
- 2026-03-27
- Publication Date
- 2026-10-01
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Figure US2026021238_01102026_PF_FP_ABST
Abstract
Description
Docket No. BLUCP027WOSYSTEMS AND METHODS FOR SAMPLE TESTING FOR BATTERY- RELATED MATERIALSINCORPORATION BY REFERENCE
[0001] A PCT Request Form is filed concurrently with this specification as part of the present application. Each application that the present application claims benefit of or priority to as identified in the concurrently filed PCT Request Form is incorporated by reference herein in their entireties and for all purposes.BACKGROUND
[0002] Solid-state primary and secondary batteries present various advantages over batteries that use liquid electrolytes. For example, in lithium-ion secondary batteries, inorganic solid-state electrolytes may be less flammable than conventional liquid organic electrolytes. Solidstate electrolytes may also present advantages of high energy densities, good cycling stabilities, and electrochemical stabilities over a range of conditions. However, there are various challenges in large scale commercialization of batteries with solid-state electrolyte separators. Various battery components may undergo testing for various reasons, such as during material selection and in preparation for manufacturing.
[0003] The background provided herein is for the purposes of generally presenting the context of the disclosure. Work of the presently named inventors, to the extent that it is described in this background, as well as aspects of the description that may not otherwise qualify as prior art at the time of filing, are neither expressly nor impliedly admitted as prior art against the disclosure.SUMMARY
[0004] Details of one or more implementations of the subject matter described in this specification are set forth in the accompanying drawings and the description below. Other features, aspects, and advantages will become apparent from the description, the drawings, and the claims. The following, non-limiting implementations are considered part of the disclosure; other implementations will be evident from the entirety of this disclosure and the accompanying drawings as well.
[0005] In some embodiments, a sample testing system includes: a mixing chamber having a first inlet, a second inlet, and an outlet; a first source of a first gas fluidically connected to the first inlet of the mixing chamber via a first flowpath, wherein the first gas and a first componentDocket No. BLUCP027WOflow from the first flowpath to the mixing chamber; a first mass flow controller (MFC) fluidically interposed along the first flowpath and configured to control the flow of the first gas to the mixing chamber; a second source of second gas fluidically connected to the second inlet of the mixing chamber via a second flowpath; a second MFC fluidically interposed along the second flowpath and configured to control the flow of the second gas to the mixing chamber; a sample chamber having a sample chamber inlet fluidically connected to the outlet of the mixing chamber by a first outlet flowpath; a first sensor configured to detect the first component inside the mixing chamber and generate data indicative of a first concentration of the first component in the mixing chamber; and a first controller communicatively connected to the first sensor and the first MFC, and configured to: receive first sensor data from the first sensor, and control, based at least in part on the first sensor data, the first MFC to control a flowrate of the first gas through the first MFC and thereby cause a first desired concentration of the first component to be in the mixing chamber, wherein a testing mixture including the first gas, the dry air, and the first component is configured to flow from the mixing chamber to the sample chamber inlet through the first outlet flowpath.
[0006] In some embodiments, the system further includes a sensor chamber fluidically connected to a sample chamber outlet of the sample chamber by a second outlet flowpath spanning from the sample chamber outlet to the sensor chamber such that gas is configured to flow from the sample chamber to the sensor chamber through the second outlet flowpath; and a second sensor coupled to the sensor chamber and configured to detect a second component in the sensor chamber and generate second sensor data indicative of a second amount of the second component in the sensor chamber.
[0007] In some embodiments, the system further includes a third sensor coupled to the sensor chamber and configured to detect the second component in the sensor chamber and generate third sensor data indicative of a third amount of the second component in the sensor chamber.
[0008] In some embodiments, the second component includes water, sulfur dioxide, sulfur vapor, oxygen, hydrogen, hydrogen sulfide, carbon dioxide, carbon monoxide.
[0009] In some embodiments, the system further includes a fourth sensor coupled to the sensor chamber and configured to detect the first component in the sensor chamber and generate fourth sensor data indicative of a fourth amount of the first component in the sensor chamber.
[0010] In some embodiments, the system further includes a first valve having a first valve inlet, a first valve outlet, and a second valve outlet, and fluidically interposed along the first outlet flowpath; a second valve having a second valve inlet, a third valve inlet, and a third valve outlet, and fluidically interposed along the second outlet flowpath; and a bypass flowpathDocket No. BLUCP027WOspanning from, and fluidically connecting, the second valve outlet of the first valve to the third valve inlet of the second valve, wherein: the sample chamber inlet is fluidically connected to the first valve outlet of the first valve, the sample chamber outlet is fluidically connected by the second outlet flowpath to the second valve inlet of the second valve, in a first configuration, the first valve is configured to cause the testing mixture flowing through the first valve inlet to flow out the first valve outlet to the sample chamber, in a second configuration, the first valve is configured to cause the testing mixture flowing through the first valve inlet to flow out the second valve outlet to the bypass flowpath, in a third configuration, the second valve is configured to cause gas flowing from the sample chamber through the third valve inlet to flow out the third valve outlet to the sensor chamber, and in a fourth configuration, the second valve is configured to cause gas flowing from the bypass flowpath through the third valve inlet to flow out the third valve outlet to the sensor chamber.
[0011] In some embodiments, when the first valve is in the first configuration and the second valve is in the third configuration, the testing mixture is caused to flow from the mixing chamber to the sample chamber, and gas including the testing mixture is caused to flow from the sample chamber to the sensor chamber.
[0012] In some embodiments, the system further includes an exhaust flowpath fluidically connected to the bypass flowpath; and an exhaust valve fluidically interposed along the exhaust flowpath and configured to control flow of gas through the exhaust flowpath, wherein gas flowing in the bypass flowpath is configured to flow to and through the exhaust flowpath when the exhaust valve is in an open position.
[0013] In some embodiments, the system further includes a third valve having a fourth valve inlet, a fifth valve inlet, and a fourth valve outlet, and fluidically interposed along the first outlet flowpath and fluidically interposed between the first valve and the sample chamber; and an inert gas source fluidically connected to the fifth valve inlet of the third valve and configured to flow the inert gas into the sample chamber, wherein: in a fifth configuration, the third valve is configured to cause gas flowing through the fourth valve inlet to flow out the fourth valve outlet and to the sample chamber, and in a sixth configuration, the third valve is configured to cause the inert gas flowing through the fifth valve inlet to flow out the fourth valve outlet and to the sample chamber.
[0014] In some embodiments, the system further includes a pressure relief valve fluidically interposed along the first outlet flowpath and interposed between the first valve and the mixing chamber.Docket No. BLUCP027WO
[0015] In some embodiments, the system further includes a second controller configured to control operation of the first valve and the second valve, and having one or more processors and one or more memories storing instructions for causing the one or more processors to cause: the first valve to be in the first configuration and the second valve to be in the fourth configuration at the same time and thereby causing the testing mixture to flow from the mixing chamber to the sample chamber, and causing gas including the testing mixture to flow from the sample chamber to the sensor chamber, and the first valve to be in the second configuration and the second valve to be in the third configuration at the same time and thereby causing the testing mixture to flow from the mixing chamber to the bypass flowpath and not to sample chamber.
[0016] In some embodiments, the system further includes a liquid source fluidically interposed along the first flowpath, wherein: the liquid includes the first component, and the first gas is configured to receive the first component from the liquid source and form a first mixture including the first gas and the first component.
[0017] In some embodiments, the liquid source is water and the first component is water.
[0018] In some embodiments, the first component is a vapor in the first gas.
[0019] In some embodiments, the first gas is dry air.
[0020] In some embodiments, the second gas is dry air.
[0021] In some embodiments, the dry air includes less than 25% oxygen, less than 5% hydrogen, less than 3% carbon dioxide, less than 3% carbon monoxide, and greater than 70% nitrogen.
[0022] In some embodiments, the system further includes a first valve having a first valve inlet, a first valve outlet, and a second valve outlet, and fluidically interposed along the first outlet flowpath; and a bypass flowpath spanning from the second valve outlet to an exhaust, wherein: the sample chamber inlet is fluidically connected to the first valve outlet, in a first configuration, the first valve is configured to cause the testing mixture flowing through the first valve inlet to flow out the first valve outlet, and in a second configuration, the first valve is configured to cause the testing mixture flowing through the first valve inlet to flow out the second valve outlet.
[0023] In some embodiments, the first valve outlet and the second valve outlet are oriented with respect to each other at less than 180 degrees.
[0024] In some embodiments, the system further includes an inert gas source fluidically connected to the sample chamber and configured to flow the inert gas into the sample chamber.Docket No. BLUCP027WO
[0025] In some embodiments, the first controller is a proportional integral derivative (PID) controller.
[0026] In some embodiments, the sample chamber: has a chamber interior, an interior inlet configured to flow gas from the sample chamber inlet into the chamber interior, and an interior outlet configured to flow gas out of the chamber interior to a sample chamber outlet, is configured to support a sample in the chamber interior at a first offset distance from the interior inlet, and is configured to support the sample in the chamber interior at a second offset distance, less than the first offset distance, from the interior inlet.
[0027] In some embodiments, at the first offset distance, the sample chamber is configured to cause gas flowing into the chamber interior to be turbulent flow, and at the second offset distance, the sample chamber is configured to cause gas flowing into the chamber interior to be diffuse flow.
[0028] In some embodiments, the system further includes a third source of a third gas fluidically connected to a third inlet of the mixing chamber via a third flowpath, wherein the third gas and a third component flow from the third flowpath to the mixing chamber; a third MFC fluidically interposed along the third flowpath and configured to control the flow of the third gas to the mixing chamber; a fifth sensor configured to detect the third component inside the mixing chamber and generate fifth sensor data indicative of a fifth concentration of the third component in the mixing chamber; and a third controller communicatively connected to the fifth sensor and the third MFC, and configured to: receive third sensor data from the fifth sensor, and control, based at least in part on the fifth sensor data, the third MFC to control a flowrate of the third gas through the third MFC and thereby cause a third desired concentration of the third component to be in the mixing chamber, wherein the testing mixture including the first gas, the second gas, the first component, the third gas, and the third component is configured to flow from the mixing chamber to the sample chamber inlet through the first outlet flowpath.
[0029] In some embodiments, the system further includes one or more temperature control apparatuses coupled to one or more of the mixing chamber, the sample chamber, one or more conduits of the first flowpath, one or more conduits of the second flowpath, or one or more conduits of the outlet flowpath, wherein: each temperature control apparatus is configured to control a temperature of the mixing chamber, the sample chamber, one or more conduits of the first flowpath, one or more conduits of the second flowpath, one or more conduits of the outlet flowpath to which it is coupled, and the temperature ranges from about 0 °C to about 150 °C.Docket No. BLUCP027WO
[0030] In some embodiments, at least one temperature control apparatus is a heater, an active cooler, or both.
[0031] In some embodiments, the system further includes one or more second temperature control apparatuses coupled to one or more of the mixing chamber, the sample chamber, one or more conduits of the first flowpath, one or more conduits of the second flowpath, or one or more conduits of the outlet flowpath, wherein: each second temperature control apparatus is configured to control a second temperature of the mixing chamber, the sample chamber, one or more conduits of the first flowpath, one or more conduits of the second flowpath, or one or more conduits of the outlet flowpath to which it is coupled, the temperature ranges from about 25 °C to about 150 °C, and the second temperature ranges from about 0 °C to about 25 °C.
[0032] In some embodiments, the system further includes the first inlet and the second inlet are positioned at a bottom portion of the mixing chamber, and the first inlet is oriented at a non-parallel angle with respect to the second inlet.
[0033] In some embodiments a method for sample testing includes: flowing, by a first mass flow controller (MFC), a first gas and a first component through a first flowpath to a first inlet of a mixing chamber; flowing, by a second MFC, a second gas through a second flowpath to a second inlet of the mixing chamber; generating first sensor data, using a first sensor configured to detect the first component inside the mixing chamber, indicative of a first concentration of the first component in the mixing chamber; controlling, based at least in part on the first sensor data, the first MFC to control the flow of first gas and the first component and thereby causing a first desired concentration of the first component to be in the mixing chamber; and flowing a testing mixture including the first gas, the second gas, and the first component from the mixing chamber to a sample chamber through a first outlet flowpath fluidically connecting the mixing chamber and the sample chamber.
[0034] In some embodiments, the method further includes flowing gas from the sample chamber to a sensor chamber through a second outlet flowpath, wherein a second sensor is coupled to the sensor chamber and configured to detect a second component in the sensor chamber and generate second sensor data indicative of a second amount of the second component in the sensor chamber; and generating the second sensor data, by the second sensor, indicative of the second amount of the second component in the sensor chamber.
[0035] In some embodiments, the first outlet flowpath further includes a first valve having a first valve inlet, a first valve outlet, and a second valve outlet, wherein a sample chamber inlet is fluidically connected to the first valve outlet, the second outlet flowpath further includes a second valve having a second valve inlet, a third valve inlet, and a third valve outlet, whereinDocket No. BLUCP027WOa sample chamber outlet is fluidically connected by the second outlet flowpath to the third valve inlet of the second valve, a bypass flowpath spans from, and fluidically connects, the second valve outlet of the first valve to the second valve inlet of the second valve, and the method further includes: flowing the testing mixture to the sample chamber and the sensor chamber, and not the bypass flowpath, by positioning the first valve in a first configuration and thereby causing the testing mixture to flow through the first valve inlet and flow out the first valve outlet to the sample chamber, and by positioning the second valve in a third configuration and thereby causing the gas flowing from the sample chamber to flow through the third valve inlet to flow out the third valve outlet to the sensor chamber; and flowing the testing mixture to the bypass flowpath and the sensor chamber, and not to the sample chamber, by positioning the first valve in a second configuration and thereby causing the testing mixture to flow through the first valve inlet to flow out the second valve outlet to the bypass flowpath, and by positioning the second valve in a fourth configuration and thereby causing gas flowing in the bypass flowpath to flow through the third valve inlet to flow out the third valve outlet to the sensor chamber.
[0036] In some embodiments, the method further includes changing the flow of the testing mixture from flowing through the bypass flowpath to flowing through the sample chamber by changing the second valve from the third configuration to the fourth configuration and changing the first valve from the second configuration to the first configuration.
[0037] In some embodiments, the method further includes opening, before or during changing the flow of the testing mixture from flowing through the bypass flowpath to flowing through the sample chamber, an exhaust valve fluidically connected to an exhaust flowpath fluidically connected to the bypass flowpath and thereby causing the testing mixture to flow from the bypass flowpath to the exhaust flowpath.
[0038] In some embodiments, changing the second valve from the third configuration to the fourth configuration occurs at the same time, or before, changing the first valve from the second configuration to the first configuration.
[0039] In some embodiments, the method further includes changing the flow of the testing mixture from flowing through the bypass flowpath to flowing through the bypass flowpath by changing the second valve from the fourth configuration to the third configuration and changing the first valve from the first configuration to the second configuration.
[0040] In some embodiments, the method further includes generating, by a third sensor coupled to the sensor chamber and configured to detect the first component in the sensor chamber, third sensor data indicative of the first component in the sensor chamber.Docket No. BLUCP027WO
[0041] In some embodiments, the method further includes flowing, by a third MFC, a third gas and a third component through a third flowpath to a third inlet of the mixing chamber; generating fifth sensor data, using a fifth sensor configured to detect the third component inside the mixing chamber, indicative of a third concentration of the third component in the mixing chamber; controlling, based at least in part on the fifth sensor data, the third MFC to control the flow of third gas and the third component and thereby causing a third desired concentration of the third component to be in the mixing chamber; and the flowing the testing mixture further includes flowing the first gas, the second gas, the first component, the third gas, and the third component from the mixing chamber to the sample chamber through the first outlet flowpath.
[0042] Additional aspects will be set forth in the detailed description which follows, and, in part, will be apparent from the disclosure, or may be learned by practice of the disclosed embodiments and / or the claimed subject matter.BRIEF DESCRIPTION OF DRAWINGS
[0043] Figure 1 depicts an example testing system in accordance with disclosed implementations.
[0044] Figure 2 depicts another example testing system in accordance with disclosed embodiments.
[0045] Figure 3A depicts yet another example testing system.
[0046] Figure 3B depicts the system of Figure 3A in first example system configuration.
[0047] Figure 3C depicts the system of Figure 3A in a second system configuration.
[0048] Figure 3D depicts the system of Figure 3A in a third system configuration.
[0049] Figure 3E depicts the system of Figure 3A in yet another configuration.
[0050] Figure 4A depicts an example sample chamber according to disclosed implementations.
[0051] Figure 4B depicts another example sample chamber according to disclosed implementations.
[0052] Figure 5 depicts another example system in accordance with disclosed implementations.
[0053] Figure 6 depicts a first example technique for sample testing.
[0054] Figure 7 depicts another example technique for sample testing.
[0055] Figure 8 depicts a mixing chamber according to disclosed implementations.
[0056] Figure 9 depicts yet another example system in accordance with disclosed implementations.Docket No. BLUCP027WODESCRIPTION
[0057] In the following description, numerous specific details are set forth in order to provide a thorough understanding of various embodiments. The disclosed embodiments may be practiced without some or all of these specific details. In other instances, well-known process operations have not been described in detail to not unnecessarily obscure the disclosed embodiments. While the disclosed embodiments will be described in conjunction with specific embodiments, it will be understood that it is not intended to limit the disclosed embodiments. Introduction and Context
[0058] Various batteries, including new and emerging batteries, use various components and chemicals and it is desirable to perform testing of these elements when selecting them for use, when developing manufacturing procedures, and assessing safety risks for making and using the batteries. For example, many battery materials are reactive with air, water, and the gaseous components of air which presents numerous challenges and complexities when using such materials. Many battery manufacturing facilities control the environment in which the battery materials are located during storage and manufacturing, such as using dehumidifying systems as well as inert gas streams to reduce moisture and oxygen levels at or near the surface of the materials. Further challenges may arise because some interactions between battery materials and air may result in competing and concurrent chemical reactions. It is therefore advantageous to determine and understand the reactions between one or more gases or components in air, like moisture, carbon dioxide, or oxygen, and battery materials. For instance, such understandings can affect which materials can be used in batteries, the safety risks associated with such materials, the amount and / or duration of time that a battery material can be exposed to the one or more gases or components, and such understandings can ultimately lead to developing the complex and capital intensive manufacturing processes.
[0059] In one example, it is beneficial to test and determine the reactivity of air at numerous humidity levels with battery-related materials, such as a sulfide solid electrolyte powder, a coated electrode having air-reactive sulfides, or a separator film having air-reactive sulfides. However, this testing and determining presents numerous challenges and complexities. For instance, air generally contains multiple reagents, such as water, oxygen, and carbon dioxide, and each reagent is capable of reacting with a sulfide, decomposition products, or both which makes quantifying the reactions very difficult. It is therefore desirable when testing and assessing such battery-related materials to provide precise control of the concentration, flowrate, or both of the various components of air in a reagent stream. This may provide the ability to quantify the reactivity of a battery-related material with air having one or moreDocket No. BLUCP027WOcontrolled components, like humidity, oxygen, or carbon dioxide. This may also provide the ability to simulate varying exposure conditions that a material may encounter in different environments, such as manufacturing, storage, maintenance, or in-use. This may further provide the ability to determine and measure reaction byproducts. For example, a sulfide solid may react with air and generate hydrogen sulfide gas, and it is desirable to measure and quantify the yield of this byproduct hydrogen sulfide gas.
[0060] Provided herein are new and novel systems and techniques for testing material samples, such as materials used in batteries. In some instances, these systems are configured to control the concentration, flow, or both, of at least one gas stream to a sample testing chamber, and to measure one or more components flowing out of the sample testing chamber. As detailed below, these systems flow two separate gas flows into a mixing chamber to create a testing mixture of the two separate gas flows. At least one of these gas flows has a component and the systems are configured to control the flow of at least one of these gas flows into the mixing chamber to create a desired concentration of the component in the mixing chamber and resulting testing mixture. This testing mixture having the desired concentration of the component is flowed to a sample chamber where a sample of material is positioned. The gases and materials in the sample chamber, such as the testing mixture and byproducts of reactions between the testing mixture and the sample of material, may be detected and measured by various sensors.
[0061] For example, a first gas having a first component is flowed into the mixing chamber and a sensor coupled to the mixing chamber is configured to detect the first component and generate first sensor data indicative of a concentration, or amount, of the first component in the mixing chamber. Based on this first sensor data, the flow of the first gas may be adjusted, such as increased, decreased, or kept constant, to result in a desired concentration of that first component in the mixing chamber. This control may be considered proportional-integral-derivative, or PID, control in which the systems use a feedback-based control loop using the sensor data and control of first gas flow to adjust and maintain the concentration of the first component at the desired setpoint, or within a particular range of the setpoint, such as within 1% or 5%. The resulting testing mixture in the mixing chamber has the first gas, the second gas, and the first component at the desired concentration, and this testing mixture is flowed to the sample chamber.
[0062] Some systems may have a second sensor configured to detect a second component, such as a reaction byproduct from the sample testing chamber, and generate sensor data indicative of a concentration, or amount, of the second component. This second sensor data may be usedDocket No. BLUCP027WOto determine the amount of that byproduct produced by a reaction of the sample with the first component at the first desired concentration. In some implementations, the systems may have a sensor chamber downstream of the sample chamber and the second sensor may be coupled to this sensor chamber. The gases and components in the sample chamber may flow to the sensor chamber where the second sensor, and other sensors, may detect one or more constituents from the sensor chamber.
[0063] In some implementations, the systems may use mass flow controllers (MFCs) to control the gas flows into the mixing chamber. Some systems may also use and flow dry air into the mixing chamber. Dry air may be considered, in some instances, a gas mixture having oxygen, hydrogen, carbon dioxide, carbon monoxide, and nitrogen, and in some cases other trace gases, and not having any moisture or water, such as about 0%. The systems may also have various flowpaths and pressure controls configured to maintain pressures in the system and prevent or reduce unwanted pressure spikes which may adversely affect the systems, such as interfering with the MFC operation, control loop in the mixing chamber, or both. For example, some systems may have a bypass flowpath fluidically connected to the mixing chamber and configured to flow the testing mixture out of the mixing chamber to another location, not into the sample chamber, in order to provide for steady state flow of the testing mixture before flowing it into the sample chamber. Various valve operation sequences may be performed to switch gas flows between the bypass flowpath and the sample chamber in order to prevent or reduce unwanted pressure changes in the system.Testing Systems and Techniques
[0064] Figure 1 depicts an example testing system in accordance with disclosed implementations. The testing system 100 has a mixing chamber 102, a first source 104, a second source 106, and a sample chamber 108. The mixing chamber 102 has a first inlet 110, a second inlet 112, and a mixing chamber outlet 114. The first source 104 contains a first gas and is fluidically connected to the first inlet 110 by a first flowpath 116. A first mass flow controller (MFC) 118 is fluidically positioned, or fluidically interposed, along the first flowpath 116 and configured to control the flow, such as the flowrate, of the first gas along the first flowpath 116 and into the mixing chamber 102. The first MFC 118 is configured to flow the first gas at various flowrates such as from about 0.5 standard cubic centimeters per minute (SCCM) to about 1 standard liter per minute (SLM). As described in more detail below, the first MFC 118 is adjustable and configured to provide variable flowrates.
[0065] In some implementations, the first gas in the first source 104 may be dry air. This dry air may have less than 25% oxygen, less than 5% hydrogen, less than 3% carbon dioxide, lessDocket No. BLUCP027WOthan 3% carbon monoxide, and greater than 70% nitrogen, for example. In one further example, the dry air may range from about 20% to about 22% oxygen, about 2% hydrogen, about 1% carbon dioxide, about 1% carbon monoxide, and about 76% nitrogen. This dry air may also have a moisture (or water) by volume that is less than 100 parts per million (ppm), less than 75 ppm, less than 50 ppm, less than 25 ppm, or less than 10 ppm, for instance.
[0066] When the first gas flows into the mixing chamber 102, a first component is also flowed with, or in, the first gas to the mixing chamber 102. The first component may be a component of the first gas itself, such as oxygen or carbon dioxide in the first gas, or the first component may be added to the first gas in the first flowpath 116. In some implementations, the first component may be added from a liquid state to the first gas along the first flowpath 116. In some instances, the liquid may be in a reservoir or other container that is absorbed by a wick positioned partially inside the reservoir and the first gas flows past the wick and liquid therein is desorbed and added to the first gas. The wick may be a porous material, such as a fiber or paper, that absorbs water from the reservoir. As the first gas flows past the wick with the liquid therein, the liquid evaporates from the wick and saturates the first gas. In another instance, the liquid having the first component may be vaporized by a vaporizer or other heater that is configured to heat and the liquid from liquid state to vapor state. The liquid source or vaporizer is depicted in Figure 1 as box 120 which is positioned along the first flowpath 116.
[0067] In some implementations, the liquid is water that is added to the first gas along the first flowpath 116. This water may be added in various manners such as by flowing the first gas past the liquid source 120 which may have water and a wick positioned partially in the water reservoir. In some examples, the liquid may be an organic solvent having one or more volatile organic compounds (VOCs), such as acetic acid or glacial acetic acid, which may be the first component. In such instances, the first sensor 126 is configured to detect and measure the one or more VOCs and the controller 130 is configured to control the first MFC 118 to control flow of the first gas to result in the desired concentration of the one or more VOCs in the mixing chamber 102. This first gas with the first component, which may be water in one example, may be considered a first mixture and this first mixture flows into the mixing chamber 102 through the first inlet 110. In Figure 1, the first gas is represented as white arrows Al, and the first gas with the first component is represented as black arrows A2.
[0068] As can be seen, once the first gas has flowed past the liquid source 120, the first gas and the water flow into the mixing chamber 102. In some implementations, the first component may be at a first concentration in the first gas when flowing into the mixing chamber 102. This first concentration may, in some instances, be constant while in other instances, it may changeDocket No. BLUCP027WOover time. As described below, the system 100 is configured to maintain a first desired concentration or amount of the first gas in the mixing chamber 102 which may be independent of the first concentration of the first component flowing into the mixing chamber 102.
[0069] The second source 106 may have a second gas which may also be dry air like the first source or the first gas. For example, the second gas may be dry air having less than 25% oxygen, less than 5% hydrogen, less than 3% carbon dioxide, less than 3% carbon monoxide, and greater than 70% nitrogen, for example. In one further example, the dry air may range from about 20% to about 22% oxygen, about 2% hydrogen, about 1% carbon dioxide, about 1% carbon monoxide, and about 76% nitrogen. This dry air may also have a moisture (or water) by volume that is less than 100 ppm, less than 75 ppm, less than 50 ppm, less than 25 ppm, or less than 10 ppm, for instance. The second source 106 is fluidically connected to the second inlet 112 by a second flowpath 122. A second MFC 124 is interposed along the second flowpath 122 and configured to control the flow of the second gas, indicated with arrows A3, to the second inlet 112 and into the mixing chamber 102. The second MFC 124 is configured to flow the second gas at various flowrates such as from about 250 SCCM SLM to about 15 SLM.
[0070] The system 100 is configured to provide a feedback control loop that controls the concentration, or amount, of the first component in the mixing chamber 102 by adjusting the flowrate of the first gas into the mixing chamber 102. As can be seen, the system 100 has a first sensor 126 coupled to the mixing chamber 102 and configured to detect the first component in the mixing chamber 102. For example, the first component may be water, or moisture or H₂O, and the first sensor 126 is configured to detect water. The first sensor 126 is further configured to generate first sensor data 128 indicative of an amount, or a concentration, of the first component in the mixing chamber 102. For example, the first sensor data may indicate the concentration in ppm of the first component in the mixing chamber. The system 100 has a controller 130 communicatively coupled to the first sensor 126 and the first MFC 118, and configured to receive the first sensor data 128 from the first sensor 126. The controller 130 is configured to control, based on the first sensor data, the MFC 118 in order to cause a first amount, or first concentration, of the first component in the mixing chamber. This control of the first MFC 118 may be controlling the flowrate of the first gas through the first MFC 118, and may be causing the flowrate of the first gas to increase, decrease, or remain constant. In some implementations, the controller is configured to cause the concentration of the first component to be within a range of the first concentration, such as within at least about 0.05%, 0.1%, 0.5%, 1%%, or 5%.Docket No. BLUCP027WO
[0071] For instance, if the detected concentration of the first component is less than the desired first concentration, then the controller 130 may cause the MFC 118 to increase the flow of the first gas which causes more moisture to flow into the mixing chamber 102 and thereby increase the concentration of the first component therein. In another instance, if the detected concentration of the first component is greater than the desired first concentration, then the controller 130 may cause the MFC 118 to decrease the flow of the first gas which causes less moisture to flow into the mixing chamber 102 and thereby decrease the concentration of the first component therein.
[0072] In some implementations, the controller 130 may be considered a proportional-integral-derivative controller, or PID controller. The PID controller may receive the first sensor data 128, calculate the difference between an actual value of the first component in the mixing chamber, such as the measured concentration or measured amount, and the desired concentration or desired amount, and then adjust or maintain the flowrate of the first MFC 118 to control the output of the first gas and first component into the mixing chamber 102. In some implementations, the controller 130 may be a controller having one or more processors and one or more memories storing instructions that are configured to cause the one or more processors to receive the first sensor data and determine a flowrate of the first gas by the first MFC 118 to cause the desired amount or concentration of the first component to be in the mixing chamber 102. This may include a programmable logic controller, or PLC, that may use programming languages such as functional block diagrams, ladder logic, and the like. Any controller referred to herein may be considered such a controller with PID, PLC, or other programming.
[0073] With the first gas, the first component, and the second gas flowing into the mixing chamber 102, a testing mixture is formed in the mixing chamber 102 having these components. This testing mixture also has the desired amount, or desired concentration, of the first component as a result of the control by the controller 130 and the control loop provided above. The testing mixture with the first gas, the first component, and the second gas flows out of the mixing chamber outlet 114 of the mixing chamber 102 and to the sample chamber 108 via a first outlet flowpath 132. In Figure 1, the testing mixture is labeled with arrows A4. The sample chamber 108 may have one or more samples of battery material positioned therein, such as sulfide powder, and the testing mixture is configured to flow into the sample chamber 108 and onto the one or more samples.
[0074] One or more reactions may, or may not, occur between the testing mixture and the one or more samples, and the system is configured to detect one or more components related to the one or more reactions. This may include detecting the one or more components, like a reactionDocket No. BLUCP027WObyproduct such as a gas or compound like oxygen, carbon dioxide, carbon monoxide, hydrogen sulfide, hydrogen, sulfur dioxide, or water, of the gases in the sample chamber with at least one additional sensor. The additional sensor may be coupled to the sample chamber 108 and configured to detect gases within the sample chamber 108, or coupled to a sensor chamber, downstream of the sample chamber 108 and configured to receive the gases from the sample chamber, and configured to detect gases within the second chamber.
[0075] As illustrated in Figure 1, the system 100 has a second sensor 134 coupled with the sample chamber 108 and configured to detect a second component in the sample chamber 108. As provided above, this second component may be a gas or compound like carbon dioxide, carbon monoxide, water, hydrogen sulfide, sulfur dioxide, hydrogen, or oxygen. The second sensor 134 is configured to generate second sensor data indicative of an amount or concentration of the second component in the sample chamber 108. This second sensor data may be received by one or more second controllers configured to receive this second sensor data and take various actions in response to such data. This may include comparing this second sensor data to a threshold value and determining whether this second sensor data indicates that the amount or concentration of the second component is above or below this threshold value. The second controller may be configured to issue a notification or transmission of information related to this second sensor data, such as the values of the second sensor data as well as the comparing and determination.
[0076] In some implementations, the system may have a sensor chamber downstream of the sample chamber that is configured to receive the gases from the sample chamber and that has one or more sensors configured to detect components in those received gases. Having a separate sensor chamber may provide various advantages, such as providing sensors in desired locations and positions for accurate sensing, as well as flexible testing conditions within the sample chamber that are independent of sensor detections. These separate chambers may also provide for more accurate detections of the gases, like reactants and byproducts, from the sample chamber. For instance, the various gases may be caused to mix together and provide a more accurate, homogenous concentration of the gases and components therein to a sensor. However, some sensors coupled to the sample chamber, depending on their position with respect to the sample chamber, may provide inaccurate detections by detecting concentrations that may be higher or lower than the component in a well-mixed gas. A sensor directly over a sample where reactions occur may detect a concentration of a byproduct that may be higher than a homogenous concentration of the gases in the sample chamber, for example. Similarly, another sensor underneath the sample in the sample chamber which may detect a concentration of theDocket No. BLUCP027WObyproduct lower than the homogenous concentration of the gases. By providing an opportunity for the gases to mix together, more accurate detections and testing may be provided using a separate sensor chamber. Further, some sensors may detect incoming components, such as the first component before a reaction occurs, which may provide for further inaccurate results.
[0077] Figure 2 depicts another example testing system in accordance with disclosed embodiments. Many of the components of system 200 are the same as system 100, except for noted differences, and the last two digits of the feature labels indicate the same features in the systems. For conciseness, these same features are not repeated. The system 200 in Figure 2 has a sensor chamber 236 fluidically connected to, and downstream of, the sample chamber 208. Gases, particulates, and other components in the sample chamber 208 are configured to flow from a sample chamber outlet 238 to the sensor chamber 236 via a second outlet flowpath 240. The sensor chamber 236 has a second sensor 234 configured to detect a second component in the sensor chamber 236, like described above with respect to the second sensor 134. For instance, this second component may be a gas or compound like carbon dioxide, carbon monoxide, water, hydrogen sulfide, sulfur dioxide, hydrogen, or oxygen, and the second sensor 234 is configured to generate second sensor data indicative of an amount or concentration of the second component in the sensor chamber 236.
[0078] As noted above, the sensor chamber may provide various benefits. For example, some sensors have various requirements, such as positioning with respect to flow direction or minimum flowrates, to enable their detecting and measuring, and the sensor chamber may advantageously provide for the sensors to be positioned and arranged so they may accurately and properly detect and measure the various components. For instance, a moisture sensor may require flow in particular direction like perpendicular, or crosswise, with respect to its sensor or sensor port, a hydrogen sulfide sensor may require stagnant flow, and another hydrogen sulfide sensor may require gas flow in a particular direction. It may therefore be challenging to provide some sensors on the sample chamber in the desired or required positions, and positioning such sensors on the sensor chamber may provide for more accurate detecting and measuring by these sensors.
[0079] In Figure 2, the system 200 may also have a third sensor 242 coupled to the sensor chamber 236 and configured to detect a third component in the sensor chamber 236. In some instances, this third component may be different than the first or second components. In some other cases, this third component may be the same as the second component. In these cases, it may be advantageous to provide two different sensors for detecting the same second component which can provide better accuracy or results. In one example, the second component may beDocket No. BLUCP027WOhydrogen sulfide and the second sensor 234 and the third sensor 242 may both be configured to detect and measure hydrogen sulfide. In other examples, the second component may be carbon dioxide, carbon monoxide, water, sulfur dioxide, hydrogen, or oxygen.
[0080] In some implementations, it may be advantageous to measure the first component at a second location downstream of the mixing chamber 202. This may provide for comparing the amount or concentration of the first component in the mixing chamber and in the sample chamber 208, or sensor chamber 236, to confirm the measurement by the first sensor and whether the first component remains at the desired amount or concentration, or within an acceptable range to that desired concentration, as the gases travel through the system. This may also provide for determining consumption of a reactant, such as the first component. For instance, the initial amount of the first concentration before flowing into the sample chamber 208 may be determined using the first sensor 226, and the amount of the first component after it has flowed through the reaction chamber 208 may be determined using this downstream sensing of the first component. The reaction rate, consumption rate, or both may be determined using these amounts from the sensors. To illustrate this, system 200 has a fourth sensor 244 coupled to the sensor chamber 236 and configured to detect the first component in the sensor chamber 236.
[0081] In one specific example, the first component may be water, and the first sensor 226 and the fourth sensor 244 may both be water sensors. The detections by both the first sensor 226 and the fourth sensor 244 may be compared with each other to make various assessments and adjustments. For instance, if the measurement by the fourth sensor 244 indicates that concentration of the first component is less than the concentration in the mixing chamber as indicated by the first sensor 226, then the amount or concentration of the first component in the mixing chamber may be increased. Conversely, if the measurement by the fourth sensor 244 indicates that concentration of the first component is greater than the concentration of the first component indicated by first sensor 226, then the amount or concentration of the first component in the mixing chamber may be decreased.
[0082] It may be advantageous to provide additional flowpaths and flow controls throughout the testing systems. For example, it may be beneficial to create a steady state flow of the testing mixture out of the mixing chamber before flowing the testing mixture into the sample chamber. It may also be beneficial to flow the testing mixture out of the mixing chamber and into the sensor chamber, without flowing it through the sample chamber, to measure the first component in the mixing chamber and the sensor chamber for calibration. Figure 3A depicts yet another example testing system. Here, the system 300 has many of the components ofDocket No. BLUCP027WOsystems 200 and 100, except for noted differences; the last two digits of the feature labels indicate the same features in the systems and for conciseness, these same features are not repeated.
[0083] In Figure 3A, the system 300 includes the first source 304, the second source 306, the mixing chamber 302, the sample chamber 308, and sensor chamber 336 which are the same as the features provided in Figure 2. The system 300 here also includes additional features, such as a bypass flowpath 346 that provides for gas to flow through the system 300 without flowing through the sample chamber 308. In this example, the bypass flowpath 346 spans between, and fluidically connects, the first outlet flowpath 332 and the second outlet flowpath 340. To provide for flow control between these flowpaths, a first valve 348 is fluidically interposed along the first outlet flowpath 332 and configured to control flow along the first outlet flowpath 332. The first valve 348 is configured to cause gas flowing from the mixing chamber outlet 314 through the first outlet flowpath 332 to continue flowing through the first outlet flowpath 332 to the sample chamber 308, or to flow to the bypass flowpath 346.
[0084] In some instances, the first valve 348 has a first valve inlet 350, a first valve outlet 352, and a second valve outlet 354. The first valve inlet 350 is fluidically connected to the mixing chamber outlet 314, the sample chamber 308 is fluidically connected to the first valve outlet 352, and the bypass flowpath 346 is fluidically connected to the second valve outlet 354. In a first configuration, illustrated in Figure 3B and discussed below, the first valve 348 is configured to flow gas to the sample chamber 308 and not the bypass flowpath 346. In a second configuration, illustrated in Figure 3C and discussed below, the first valve 348 is configured to flow gas to the bypass flowpath 346 and not to the sample chamber 308.
[0085] Similarly, a second valve 356 is fluidically interposed along the second outlet flowpath 340 and configured to control flow along the second outlet flowpath 340. The second valve 356 is configured to cause gas flowing from the sample chamber outlet 338 through the second outlet flowpath 340 to flow to the sensor chamber 336, or to cause gas flowing from the bypass flowpath 346 to flow to the sensor chamber 336. In some instances, the second valve 356 has a second valve inlet 358, a third valve inlet 360, and a third valve outlet 362. The second valve inlet 358 is fluidically connected to the sample chamber outlet 338, the bypass flowpath 346 is fluidically connected to the third valve inlet 360, and the third valve outlet 362 is fluidically connected to the sensor chamber 336. In a third configuration, illustrated in Figure 3B and discussed below, the second valve 356 is configured to flow gas from the sample chamber 308, not from the bypass flowpath 346, to the sensor chamber 336. In a fourth configuration,Docket No. BLUCP027WOillustrated in Figure 3C and discussed below, the second valve 356 is configured to flow gas from the bypass flowpath 346, not from the sample chamber 308, to the sensor chamber 336.
[0086] Flow control with the bypass flowpath and system 300 is illustrated in Figures 3B and 3C. In Figure 3B, the system of Figure 3A is depicted in a first system configuration. Here, the first valve 348 is in the first configuration and the second valve 356 is in the third configuration. In the first configuration, the first valve inlet 350 and the first valve outlet 352 are open, as indicated by them having no shading, and the second valve outlet 354 is closed, as indicated by it having dark shading. Gas is configured to flow from the mixing chamber 302, through the mixing chamber outlet 314, and through the first outlet flowpath 332 to the sample chamber 308, as indicated by arrows A4. Gas does not flow out of the second valve outlet 354 to the bypass flowpath 346. In the third configuration, the second valve inlet 358 and the third valve outlet 362 are open, as indicated by them having no shading, and the third valve inlet 360 is closed, as indicated by it having dark shading. Gas is configured to flow from the sample chamber 308, through the sample chamber outlet 338, and through the second outlet flowpath 340 to the sensor chamber 336, as indicated by arrows A4. Gas thereby flows through the second valve inlet 358 and the third valve outlet 362 of the second valve 356. This configuration provides for gas, such as the testing mixture in the mixing chamber 302, to flow into the sample chamber 308, out of the sample chamber 308 and through the second outlet flowpath 340 to the sensor chamber 336.
[0087] In Figure 3C, the system of Figure 3A is depicted in a second system configuration. Here, the first valve 348 is in the second configuration and the second valve 356 is in the fourth configuration. In the second configuration, the first valve inlet 350 and the second valve outlet 354 are open, and the first valve outlet 352 is closed, as indicated by it having dark shading. Gas is configured to flow from the mixing chamber 302, through the mixing chamber outlet 314, and through a portion of the first outlet flowpath 332, then to the bypass flowpath 346, and not to the sample chamber 308, as indicated by arrows A5. In the fourth configuration, the third valve inlet 360 and the third valve outlet 362 of the second valve 356 are open, and the second valve inlet 358 is closed, as indicated by it having dark shading. Gas is configured to flow from the bypass flowpath 346, and through a portion of the second outlet flowpath 340 to the second chamber 336, as indicated by arrows A5. Gas thereby flows through the third valve inlet 360 and the third valve outlet 362 of the second valve 356. This configuration provides for gas, such as the testing mixture in the mixing chamber 302, to bypass, or not flow into, the sample chamber 308. This may allow the pressure in the system to stabilize or reach a steady state before the testing mixture is flowed to the sample chamber 308.Docket No. BLUCP027WO
[0088] In some implementations, the system may have an exhaust flowpath configured to flow gas out of the system to an exhaust. This may advantageously provide for pressure relief while switching valves as well as flowing gas out of the system for safety purposes, after testing, or during initial startup and pressure equalization. Referring back to Figure 3A, the system 300 includes an exhaust flowpath 364 fluidically connected to the bypass flowpath 346 and to an exhaust 368. The exhaust flowpath 364 also has an exhaust valve 366 configured to control the flow of gas along the exhaust flowpath 364. The system 300 may be configured to flow gases from the bypass flowpath 346 to the exhaust 368. Figure 3D depicts the system of Figure 3A in a third system configuration. Here, the first valve 348 is in the second configuration, like in Figure 3C, to flow the gas from the first valve inlet 350 to the bypass flowpath 346, and the second valve 356 is in the third configuration in which the third valve inlet 360 is closed. Here, the gas is configured to flow into the bypass flowpath 346 from the first valve 348 and not out of the bypass flowpath 346 to second valve 356. The gas flows out of the exhaust flowpath 364 with the exhaust valve 366 in an open position.
[0089] In some implementations, the system may have an inert gas source fluidically connected to one or more flowpaths. The inert gas may be flowed into the system to flush and remove gases, particulates, and other material from the system. The inert gas may be argon, dry argon, nitrogen, or dry nitrogen. For example, dry nitrogen may be at least 99% nitrogen, 99.9% nitrogen, 99.99% nitrogen, 99.999% nitrogen, 99.9999% nitrogen, or 99.99999% nitrogen. Referring back to Figure 3A, the system 300 has an inert gas source 370 fluidically connected to a fourth valve 372 fluidically interposed along the first outlet flowpath 332. The fourth valve 372 is another three-way valve and it is configured to allow inert gas to flow into the first outlet flowpath 332 and flow to the sample chamber 308, to the bypass flowpath 346, or both. The fourth valve 372 has a fourth valve inlet 374 fluidically connected to the first outlet flowpath 332 and the first valve 348, such as the first valve outlet 352. The fourth valve 372 also has a fifth valve inlet 376 fluidically connected to the inert gas 370, and a fourth valve outlet 378 fluidically connected to the first outlet flowpath 332 and the sample chamber 308.
[0090] The fourth valve 372 is also configured to allow gas flowing through the first outlet flowpath 332 to flow through the valve and to the sample chamber 308. Referring back to Figure 3B, this fourth valve is in a fifth configuration which allows gas flowing along the first outlet flowpath 332 to flow through the fourth valve inlet 374 and out the fourth valve outlet 378 to the sample chamber 308. In some instances, it may be advantageous to flow the inert gas to the sample chamber 308 while, at the same time, flowing the testing mixture through the bypass flowpath 346. This may allow for the sample chamber 308, as well as the sensorDocket No. BLUCP027WOchamber 336, to be cleared of various gases and constituents without stopping the flow of the testing mixture from the mixing chamber 302, and this flowing may be performed before or after the testing mixture is flowed to the sample chamber 308 for testing.
[0091] Figure 3E depicts the system of Figure 3 A in yet another configuration. Here, the first valve 348 is in the second configuration thereby directing the testing mixture flow to the bypass flowpath 346, as indicated by arrows A5. The exhaust valve 366 is also open and the second valve 356 is in the fourth configuration, thereby causing the testing mixture to flow from the mixing chamber 302 to the bypass flowpath 346 and out the exhaust 368. For the inert gas, the fourth valve 372 is in a sixth configuration in which the inert gas may flow through the fourth valve 372, into the first outlet flowpath 332, and into the sample chamber 308. Here, the fourth valve inlet 374 is closed and the fifth valve inlet 376 is open thereby allowing the inert gas, indicated by arrows A6, to flow out of the fourth valve outlet 378 and into the first outlet flowpath 332. This may advantageously flow the gases and other materials inside the sample chamber 308 out of the sample chamber and provide an inert air environment in the sample chamber 308. This inert air environment may provide for more accurate testing of the samples by removing unwanted gases and materials.
[0092] In some instances, the inert gas may also be flowed into the sensor chamber 336 to provide an inert air environment therein. This inert gas may be flowed into the sensor chamber 336 by having the second valve 356 in the third configuration, as illustrated. These configurations provide for the inert gas to flow from the sample chamber 308 into the sensor chamber 336. In some other instances, the second valve 356 may be in a different configuration in which the second valve inlet 358 and third valve inlet 360 are both open, and the third valve outlet 362 is closed, thereby causing the inert gas flowing out of the sample chamber 308 to flow out through a portion of the second outlet flowpath 340 and into the bypass flowpath 346. This gas may then be flowed out of the exhaust flowpath 364.
[0093] In some instances, pressure changes in the systems may have adverse effects. For instance, the first and second MFCs operate on a pressure differential, and downstream pressure increases or decreases may cause the MFCs to flow more or less gas than desired. In another instance, pressure increases or decreases downstream of the mixing chamber may change the pressure inside the mixing chamber which may change the concentration or amount of the first component in the testing mixture, which may lead to inaccurate testing results. These pressure changes may also result in unwanted condensation of components in the gases which can adversely affect the system and testing. For example, when flowing water vapor to the sampleDocket No. BLUCP027WOchamber, pressure fluctuations can cause the water vapor to condense to liquid water which can adversely affect valve or MFC operation, as well as test results.
[0094] It is therefore desirable to reduce or prevent pressure fluctuations in the system. In some implementations, the systems herein may have one or more pressure relief valves. This may include a pressure relief valve fluidically positioned along the first outlet flowpath, such as fluidically interposed between the mixing chamber and the sample chamber. For example, referring back to Figure 2, the system 200 has a pressure relief valve 280 positioned along the first outlet flowpath 232 and configured to prevent the first outlet flowpath 232 from reaching a pressure above a pressure threshold. In another example, the system 300 of Figure 300 also has a pressure relief valve 380 positioned along the first outlet flowpath 332 and fluidically interposed between the first valve 348 and the mixing chamber 302. When switching valves between different configurations, they may block gas flow and cause pressure increases upstream of the valves and cause the aforementioned adverse effects. The pressure relief valve upstream of the valves can advantageously relieve such pressure increases.
[0095] As provided below, various techniques may be employed to switch the positions and configurations of the valves to flow gases within the system, and these may reduce or prevent pressure fluctuations in the system. In some implementations, the systems may have a second controller 325 configured to control aspects of the system, such as valve operations. Referring to Figure 3A, this second controller 325 may include one or more memory devices 327, one or more mass storage devices 329, and one or more processors 431. Each processor 431 may include a central processing unit (CPU) or computer, analog, and / or digital input / output connections, stepper motor controller boards, etc. In one example, the instructions may be configured to cause the one or more processors to control the first valve 348 and the second valve 356 to be in the configurations of Figure 3B and thereby cause the testing mixture to flow to the sample chamber 308 and not the bypass flowpath 346. This may include causing the one or more processors to cause the first valve 348 to be in the first configuration and cause the second valve 356 to be in the third configuration at the same time. The instructions may further be configured to cause the one or more processors to control the first valve 348 and the second valve 356 to be in the configurations of Figure 3C and thereby cause the testing mixture to flow to bypass flowpath 346 and not the sample chamber 308. This may include causing the one or more processors to cause the first valve 348 to be in the second configuration and cause the second valve 356 to be in the fourth configuration, like depicted. This may also include switching the first and second valves between configurations at the same time, such as switching the first valve from the first configuration to the second configuration at the sameDocket No. BLUCP027WOtime as switching the second valve from the third configuration to the fourth configuration. Additional features of the control by the second controller and the techniques are provided farther below.
[0096] The valves provided herein may have various configurations and operability that provide advantages. This may include having a plurality of ports that include one or more inlets and one or more outlets, and being configured to open and close these various inlets and outlets. For example, the first valve 348 may be considered a three-way valve which has a first valve inlet 350 and the two valve outlets 352 and 354. The first valve 348 is configured to have each of these elements open or closed independent of the others. The first valve inlet 350 may be open or closed while the first valve outlet 352 is open or closed and while the second valve outlet 354 is open or closed. Similarly, the first valve outlet 352 may be open or closed while the first valve inlet 350 is open or closed and while the second valve outlet 354 is open or closed. These configurations and operability of the first valve 348 may be the same for the second valve 356 and the fourth valve 372, and such configurations and operability provide for wide-ranging flow control within the system.
[0097] In some implementations, the valves may be configured such that the one or more valve inlets and one or more valve outlets may be oriented at various angles with respect to each other. For example, the first valve outlet 352 and the second valve outlet 354 may be oriented at an obtuse angle, ranging between 90 degrees and 180 degrees, or at about 90 degrees, with respect to each other. These angles may advantageously reduce or prevent pressure fluctuations when switching the first valve 348 between causing gas to flow out of the first valve outlet 352 or the second valve outlet 354. For the second valve 356, the two valve inlets 358 and 360 may also be oriented at an obtuse angle, ranging between 90 degrees and 180 degrees, or at about 90 degrees, with respect to each other. Similarly, the two valve inlets 374 and 376 of the fourth valve 372 may be oriented at an obtuse angle, ranging between 90 degrees and 180 degrees, or at about 90 degrees, with respect to each other. Again, these angles may advantageously reduce or prevent pressure fluctuations when switching between the valve inlets of the second valve 356 and the fourth valve 372.
[0098] In some implementations, the sample chamber may be configured to provide various flow characteristics of the testing mixture onto the sample. Figure 4A depicts an example sample chamber according to disclosed implementations. The sample chamber 408 has a sample chamber inlet 437, the sample chamber outlet 438, a chamber interior 482, an interior inlet 484, an interior outlet 486, and a sample support position 488. The sample chamber 408 defines the chamber interior 482 which may be considered a plenum volume. The sampleDocket No. BLUCP027WOchamber inlet 437 may be an exterior inlet of the sample chamber 408 where the gas is received from the first outlet flowpath and the interior inlet 484 may be considered the location where the gas enters the chamber interior 482. In some instances, the interior inlet 484 may partially define the chamber interior 482, and a chamber wall 490 may be interposed between the sample chamber inlet 437 and the interior inlet 484. Gas is configured to flow from the sample chamber inlet 437 to the interior inlet 484 and then into the chamber interior 482, as illustrated with arrows A4.
[0099] Similarly, the sample chamber outlet 438 may be an exterior outlet of the sample chamber 408 where the gas flows to the second outlet flowpath and the interior outlet 486 may be considered the location where the gas exits the chamber interior 482. In some instances, the interior outlet 486 may partially define the chamber interior 482, and the chamber wall 490 may be interposed between the sample chamber outlet 438 and the interior outlet 486. Gas is configured to flow from the chamber interior 482, through the interior outlet 486, and out of the sample chamber outlet 438, as illustrated with arrows A5.
[0100] The sample support position 488 may be positioned within the chamber interior in order to provide various flow characteristics to the sample 492 on the sample support position 488. For instance, the vertical offset of the sample support position 488 from the interior inlet 484, interior outlet 486, or both may affect the flow of the gas inside the chamber interior 482. When the sample support position 488 is vertically offset from the interior inlet 484 by a relatively small distance, the gas A4 flowing into the chamber interior 482 is caused to have laminar or diffuse flow characteristics. In Figure 4A, the sample support position 488 is vertically offset from the interior inlet 484 by a first offset distance OD1 and vertically offset from the interior outlet 486 by the first offset distance OD1. This first offset distance OD1 is configured to cause the gas A4 flowing into the chamber interior 482 through the interior inlet 484 to have laminar or diffuse flow characteristics.
[0101] When the sample support position is vertically offset from the interior inlet by a relatively large distance, the gas flowing into the chamber interior is caused to have turbulent or convective flow characteristics. Figure 4B depicts another example sample chamber according to disclosed implementations. Here, the sample support position 488 is vertically offset from the interior inlet 484 by a second offset distance OD2 and vertically offset from the interior outlet 486 by the second offset distance OD2. This second offset distance OD2 is larger than the first offset distance OD1 and is configured to cause the gas A4 flowing into the chamber interior 482 through the interior inlet 484 to have turbulent or convective flow characteristics. The sample chamber provided herein is therefore configured to position theDocket No. BLUCP027WOsample in at least two locations relative to the interior inlet, interior outlet, or both in order to provide different flow characteristics of the testing mixture in the chamber interior. For instance, the sample chamber 408 of Figures 4A and 4B may be the same sample chamber 408 with the sample support position 488 at different locations in the chamber interior 482. This may provide for multiple testing capabilities of the sample 492 which can provide various testing scenarios for battery-related materials.
[0102] In some implementations, the systems provided herein may have more than one gas source or component flowed into the mixing chamber and additional control loops for controlling the amount of this additional gas or component in the mixing chamber. Figure 5 depicts another example system in accordance with disclosed implementations. Here, the system 500 has the same aspects of system 200 plus a third source 504A that contains a third gas and is fluidically connected to a third inlet 510A of the mixing chamber 202 by a third flowpath 516A. A third MFC 518A is fluidically positioned, or fluidically interposed, along the third flowpath 516A and configured to control the flow, such as the flowrate, of the third gas along the third flowpath 516A and into the mixing chamber 202. This third gas flow is illustrated with arrows labeled A5. The third MFC 518A is configured to flow the third gas at various flowrates such as from about 0.5 SCCM to about 150 SCCM. Like described herein, the third MFC 518A is adjustable and configured to provide variable flows.
[0103] In some implementations, the third gas may have a third component, such as carbon dioxide, carbon monoxide, water, hydrogen sulfide, sulfur dioxide, hydrogen, or oxygen, or other component therein. In some implementations, the third component may be at a third concentration in the third gas when flowing into the mixing chamber 202. This third concentration may, in some instances, be constant while in other instances, it may change over time.
[0104] The system 500 is configured to provide a second feedback control loop that controls the amount of the third component in the mixing chamber 202 by adjusting the flowrate of the third gas into the mixing chamber 202. As can be seen, the system 500 has a fifth sensor 526A coupled to the mixing chamber 202 and configured to detect the third component in the mixing chamber 202. For example, the third component may be carbon dioxide and the fifth sensor 526 A is configured to detect carbon dioxide. The fifth sensor 526 A is further configured to generate fifth sensor data 528A indicative of an amount, or a concentration, of the third component in the mixing chamber 202. The system 500 has a third controller 530A communicatively coupled to the fifth sensor 526A and the third MFC 518A, and configured to receive the fifth sensor data 528A from the fifth sensor 526A. The third controller 530A isDocket No. BLUCP027WOconfigured to control, based on the fifth sensor data, the third MFC 518A in order to cause a third amount, or third concentration, of the third component in the mixing chamber 202, or to cause the third amount to be within a particular range of the desired third amount, such as within 0.01%, 0.1%, 0.5%, 1%, or 5%. This control of the third MFC 518A may be controlling the flowrate of the third gas through the third MFC 518A, and may be causing the flowrate of the third gas to increase, decrease, or remain constant. The third controller 530A may be any controller provided herein, such as a PID controller. Although this third source is illustrated in Figure 5 with system 500, this third source may be provided with any system herein, such as systems 100 and 300.
[0105] In some implementations, the mixing chamber may have various configurations configured to promote mixing of gases therein and provide for accurate sensing of the components therein. These configurations may include the positioning of the first and second inlets, such as causing the inlet flows to intersect with each other. For instance, the first inlet may be positioned perpendicular to the second inlet such that the first gas and second gas flow into the mixing chamber at directions perpendicular to each other. This may be considered injecting one gas into another gas. Having these flows intersect each other may advantageously provide for mixing of the gases. One example configuration is illustrated in Figure 8 which depicts a mixing chamber according to disclosed implementations.
[0106] The mixing chamber 802 may be a mixing chamber of any system provided herein. In this instance, the first inlet 810 and second inlet 812 are both positioned in the same portion, such as the bottom portion 821, of the mixing chamber 802. The first inlet 810 is oriented at a non-parallel angle with respect to the second inlet 812 which may be, in some instances like shown, perpendicular or about 90 degrees. This orientation of the two inlets causes their respective gases to intersect with each other. For example, the first gas and first component A2 flow into the second gas A3. The first gas having the first component, illustrated in black arrows A2, flows through the first inlet 810 at a first direction DI into the interior 823 of the mixing chamber 802 and the second gas, illustrated in white arrows A3, flows through the second inlet 812 into the interior 823 at a second direction D2 oriented at a non-parallel angle to the first direction DI. The first direction DI and second direction D2 may be at various angles with respect to each other, such as perpendicular, acute, or between about 15 degrees and 135 degrees. The first gas with the first component and the second gas are advantageously caused to intersect and mix with each other. These gases mix within the interior 823 to result in a relatively well-mixed, homogenous testing mixture of the first gas, second gas, and first component, and this testing mixture A4 flows out of the outlet 814 to other parts of the system.Docket No. BLUCP027WO
[0107] In some instances, the first sensor 826 may be positioned in various locations to provide for accurate sensing of the first component in the mixing chamber 802. This may include a location opposite the second inlet 812 or a location opposite the bottom portion 821, such as a top portion 825 of the mixing chamber 802. This positioning may provide for accurate sensing of the concentration of the first component in the mixing chamber interior 823 by allowing the first gas, first component, and second gas to mix together before reaching the first sensor 826.
[0108] As noted above, various techniques for sample testing are provided herein. Figure 6 depicts a first example technique for sample testing. In block 601 of technique 600, a first gas and a first component are flowed by a first MFC through a first flowpath to a first inlet of a mixing chamber. Referring to Figure 1, for example, this refers to flowing the first gas Al from the first source 104 and the first component along the first flowpath 116, through the first inlet 110, and into the mixing chamber. As provided above, the first component may be added to the first gas, like adding the first component in a vapor state with a liquid source or vaporizer 120, or it may be in the first gas in the first source 104. This may also include flowing the first gas and first component as illustrated in systems 200, 300, and 500.
[0109] In block 603, dry air is flowed by a second MFC through a second flowpath to a second inlet of the mixing chamber. Referring back to Figure 1, this refers to flowing the second gas A3 from the second source 106, which is dry air in this example, through the second flowpath 122 and into the mixing chamber 102 through the second inlet 112.
[0110] Technique 600 also includes aspects of the control loop described above. In block 605, the first sensor data is generated using a first sensor configured to detect the first component inside the mixing chamber, with the first sensor data indicative of a first amount or concentration of the first component in the mixing chamber. In Figure 1, this refers to the first sensor 126 coupled to the mixing chamber 102 and generating the first sensor data 128 which indicates the amount or concentration of the first component, such as water, inside the mixing chamber 102. This first sensor data 128 is transmitted to the controller 130 which is configured to control the flow of the first gas into the mixing chamber 102 to cause a desired amount of the first component to be in the mixing chamber, as indicated in block 607. This control may be PID control, provided herein.
[0111] In block 609, the testing mixture having the first gas, the second gas, and the first component is flowed to a sample chamber through a first outlet flowpath. Referring back to Figure 1, this refers to flowing the testing mixture A4 through the first outlet flowpath 132 to the sample chamber 108 for use in testing one or more battery-related materials.Docket No. BLUCP027WO
[0112] As provided above, one or more sensors may detect elements in the gases and components in the sample chamber. This detection may occur in the sample chamber, like illustrated in Figure 1, or it may occur in the sensor chamber downstream of the sample chamber, like depicted in Figures 2-3 A, and 5. The technique 600 of Figure 6 includes one option of this detection in block 609 which flows the gas from the sample chamber to the sensor chamber through a second outlet flowpath. As illustrated in Figure 2 and described above, for example, the sensor chamber 236 has a second sensor 234 configured to detect a second component in the sensor chamber 236 and generate second sensor data indicative of a second amount of the second component in the sensor chamber 236. In block 613, the second sensor generates the second data indicative of the second amount of the second component in the sensor chamber 236.
[0113] Some techniques provided herein may include flowing gas through the sample chamber and through a bypass flowpath. Figure 7 depicts another example technique for sample testing. Here, blocks 701-707 are the same as blocks 601-607 described above. Block 709 of technique 700 may be similar to block 609, and include additional elements, such as placing valves into various configurations. For example, block 709 may include configuring the system 300 as shown in Figure 3B in which the first valve 348 is in the first configuration. This allows for the gas to flow from the mixing chamber 302, through the first outlet flowpath 332, through the first valve inlet 350, out the first valve outlet 352, and into the sample chamber 308. This also prevents gas from flowing into the bypass flowpath. In block 711, the gas is flowed out the sample chamber outlet 338 to the sensor chamber 336 through the second outlet flowpath 340. This includes the second valve 356 being in the third configuration in which the second valve inlet 358 and third valve outlet 362 are both open.
[0114] In block 713, gas is flowed to the bypass flowpath and not to the sample chamber, like illustrated in Figure 3C. This may include positioning the first valve in the second configuration such that gas flows into the first valve inlet 350 and out the second valve outlet 354 and into the bypass flowpath 346. This may also include positioning the second valve 356 in the fourth configuration such that gas flows into the third valve inlet 360 and out the third valve outlet 362. In some other implementations, this may include flowing the gas out of the exhaust, like illustrated in Figure 3D.
[0115] In some implementations, blocks 711 and 713 may be alternated, repeated, or performed in different orders to divert the flow of testing mixture to the sample chamber or bypass flowpath. For example, the testing mixture flowing through the bypass flowpath like in Figure 3C may be changed to the flow in Figure 3B by changing second valve 356 from theDocket No. BLUCP027WOfourth configuration to the third configuration, and changing the first valve 348 from the second configuration to the first configuration. In some instances, block 713 may be performed before block 711 and this may cause the pressure in the system 300 and flow of the testing mixture to stabilize or reach a relative constant or steady state status thereby reducing unwanted pressure fluctuations before flowing the testing mixture to the sample chamber. In some cases, the first and second valves may be changed to their respective configurations at the same time. In other cases, the second valve may be changed before the first valve.
[0116] In some implementations, when changing gas flow from the bypass flowpath to the sample chamber, the exhaust valve may also be used. For instance, block 713 may be performed in which the gas is flowed through the bypass flowpath and not into the sample chamber, like illustrated in Figure 3C. After this, the exhaust valve 366 may be opened which allows the testing mixture to flow out of the bypass flowpath 346 and into the exhaust flowpath 364 and to the exhaust 368. While this testing mixture is flowing out of the bypass flowpath 346 and into the exhaust flowpath 364, the second valve 356 may be changed from the fourth configuration to the third configuration and this operation may have limited to no effect on the pressure in the system 300 because gas is not encountering this second valve. Next, the first valve 348 may be changed from the second configuration in Figures 3C and 3D to the first configuration of Figure 3B which causes the testing mixture to flow to the sample chamber 308. This sequence of valve operations may reduce or prevent unwanted pressure fluctuations in the system.
[0117] Although not illustrated in Figures 6 or 7, some techniques may generate sensor data of the first component in the mixing chamber 302 and the sensor chamber 336 using two sensors. As stated above, like in Figure 2, system 200 has a first sensor 226 configured to generate sensor data indicative of the amount or concentration of the first component in the mixing chamber 302, and it has a fourth sensor 244 coupled to the sensor chamber 236 and configured to detect the first component in the sensor chamber 236. The techniques may adjust the flow of the first MFC 218 to reduce the difference or gap between the concentration of the first component in the mixing chamber 302 and the concentration of the first component in the sensor chamber 336.
[0118] In some implementations, the systems may have temperature control apparatuses positioned on aspects of the systems, such as on the conduits of one or more flowpaths, the mixing chamber, the sample chamber, the sensor chamber, or a combination thereof. The temperature control apparatuses may be heaters, active coolers, or both. These temperature control apparatuses may provide various advantages such as preventing unwantedDocket No. BLUCP027WOcondensation of materials, promoting mixing, simulating various experimental conditions, determining reactivity and functionality at different temperatures, or a combination thereof. A system having one or more temperature control apparatuses is illustrated in Figure 9 which depicts yet another example system in accordance with disclosed implementations. This system 900 in Figure 9 is the same system 300 in Figure 3A except for noted differences, and some labels have been removed for clarity.
[0119] System 900 has one or more temperature control apparatuses on various features and in this example, a first temperature control apparatus 951 A is positioned on the sample chamber 302 and configured to heat or actively cool the mixing chamber 302 and its interior to one or more temperatures. Although the first temperature control apparatus 951 A is depicted at the bottom of the mixing chamber 302, its location is not so limited; the first temperature control apparatus 951 A may be positioned in various locations on or around the mixing chamber 302, such as on or wrapping around the sides, top, and / or bottom of the mixing chamber 302.
[0120] In some implementations, the first temperature control apparatus 951 A may be a heater that has one or more resistive heating elements, one or more inductive heating elements, or one or more fluid conduits configured to flow a heat transfer fluid therethrough. In some such cases, the one or more temperatures may range from about 25 °C to about 150 °C. In some implementations, the first temperature control apparatus 951 A may be an active cooler, like a chiller, configured to flow a heat transfer fluid through one or more fluid conduits in contact with the mixing chamber 302. In some such cases, the one or more temperatures may range from about 0 °C to about 25 °C. When the temperature control apparatus has one or more fluid conduits through which a heat transfer fluid may flow, the temperature control apparatus may act as both a heater and active cooler by flowing heat transfer fluids at different temperatures through the one or more fluid conduits. For example, a heat transfer fluid at a first temperature ranging from about 25 °C to about 150 °C may be flowed through the first temperature control apparatus 951 A to heat the mixing chamber 302. A second heat transfer fluid at a second temperature ranging from about -25 °C to about 25 °C may be flowed through the first temperature control apparatus 951 A to actively cool the mixing chamber 302.
[0121] The system 900 may also have a feedback control loop for controlling the temperature of the first temperature control apparatus 951 A, such as PID or PLC control. This feedback control loop may have a first temperature sensor 953 A configured to detect the temperature inside the mixing chamber 302 and generate temperature sensor data indicative of the temperature inside the mixing chamber 302, and a controller 930B. The controller 930B is configured to receive the temperature data generated by the first temperature sensor 953A andDocket No. BLUCP027WOto control the first temperature control apparatus 951 A in order to cause the temperature inside the mixing chamber 302 to be at a particular temperature, or within a range of the particular temperature such as within about 1%, 5%, 10%, or 20%. As provided above, these temperatures may range from about 0 °C to about 25 °C, about 0 °C to about 150 °C, or about 25 °C to about 150 °C.
[0122] In some implementations, the system 900 may have two temperature control apparatuses on the mixing chamber 302, such as a heater and an active cooler. Here, system 900 includes a first temperature control apparatus 951 A, which may be a heater, and another temperature control apparatus 955A which may be an active cooler. Having two such temperature control apparatuses may provide for broader temperature control of the testing mixture for various experiments. Similar to above, the system 900 may be configured to provide active control of the first temperature control apparatus 951 A and the other temperature control apparatus 955A, such as by PID or PLC control using the first temperature sensor 953A.
[0123] In some implementations, the system 900 may have additional temperature control apparatuses and corresponding control loops for active control of the additional temperature control apparatus. This may include additional heaters, active coolers, or both. For example, system 900 has a second temperature control apparatus 951B coupled to the sample chamber 308 and configured to heat, actively cool, or both, the sample chamber 308 and its interior, including the sample positioned therein, to one or more temperatures that may range from about 25 °C to about 150 °C, from about 0 °C to about 25 °C, or from about 0 °C to about 150 °C. Although the second temperature control apparatus 951B is depicted at the bottom of the sample chamber 308, it may be placed in various locations on or around the sample chamber 308, such as on or wrapping around the sides, top, and / or bottom.
[0124] In some implementations, the second temperature control apparatus 951B is a heater, like provided above, and configured to heat the sample chamber 308. In some other implementations, the second temperature control apparatus 951B may be an active cooler configured to actively cool the sample chamber 308. In some other implementations the second temperature control apparatus 951B may be both a heater and active cooler, like described above. In some instances, the second temperature control apparatus 951B may be a heater and another temperature control apparatus 955B that is an active cooler may be coupled to the sample chamber 308 thereby providing both active heating and cooling of the sample chamber 308.
[0125] The system 900 may also have another feedback control loop for controlling the temperature of the second temperature control apparatus 951B, such as using PID or PLCDocket No. BLUCP027WOcontrol. This feedback control loop may have a second temperature sensor 953B configured to detect the temperature inside the sample chamber 308 and generate temperature sensor data indicative of the temperature inside the sample chamber 308, and a controller 930C. The controller 930C is configured to receive the temperature data generated by the second temperature sensor 953B and to control the second temperature control apparatus 951B in order to cause the temperature inside the sample chamber 308 to be at a particular temperature, or within a range of the particular temperature such as within about 1%, 5%, 10%, or 20%. In the instances having both the second temperature control apparatus 951B that is a heater and another temperature control apparatus 955B that is an active cooler, the system 900 is configured to provide active control of both apparatuses 951B and 955B, like described herein.
[0126] In another example, system 900 has a third temperature control apparatus 951C coupled to the sensor chamber 336 and configured to heat, actively cool, or both, the sensor chamber 336 and its interior to one or more temperatures that may range from about 25 °C to about 150 °C, from about 0 °C to about 25 °C, or from about 0 °C to about 150 °C. Although the third temperature control apparatus 951C is depicted at the bottom of the sensor chamber 336, it may be placed in various locations on or around the sensor chamber 336, such as on or wrapping around the sides, top, and / or bottom. In some implementations, the third temperature control apparatus 951C is a heater, like provided above, and configured to heat the sensor chamber 336. In some other implementations, the third temperature control apparatus 951C may be an active cooler configured to actively cool the sensor chamber 336. In some other implementations the third temperature control apparatus 951C may be both a heater and active cooler, like described above. In some instances, the third temperature control apparatus 951C may be a heater and another temperature control apparatus 955 C that is an active cooler may be coupled to the sensor chamber 336 thereby providing both active heating and cooling of the sensor chamber 336. In the instances having both the third temperature control apparatus 951C that is a heater and another temperature control apparatus 955 C that is an active cooler, the system 900 is configured to provide active control of both apparatuses 951C and 955C, like described herein.
[0127] One or more conduits of the flowpaths in the system 900 may also have temperature control apparatuses configured to heat, actively cool, or both, the respective conduits to one or more temperatures that may range from about 25 °C to about 150 °C, from about 0 °C to about 25 °C, or from about 0 °C to about 150 °C. In this example, each flowpath has a representative temperature control apparatus indicating that the one or more conduits of the respective flowpath may be heated, actively cooled, or both. As can be seen, the first flowpath 316 has aDocket No. BLUCP027WOfourth temperature control apparatus 951D configured to heat, actively cool, or both the one or more conduits of the first flowpath 316, the second flowpath 322 has a fourth temperature control apparatus 951E configured to heat, actively cool, or both, the one or more conduits of the second flowpath 322, the first outlet flowpath 332 has a fifth temperature control apparatus 951F configured to heat, actively cool, or both, the one or more conduits of the first outlet flowpath 332, the second outlet flowpath 340 has a sixth temperature control apparatus 951G configured to heat, actively cool, or both, the one or more conduits of the second outlet flowpath 340, and the bypass flowpath 346 has a seventh temperature control apparatus 951H configured to heat the one or more conduits of the bypass flowpath 346. Although a single temperature control apparatus is identified for each flowpath, more than one temperature control apparatus may be used.
[0128] In some instances, these temperature control apparatuses 951D-951H may be heaters, like provided above, and configured to heat the respective conduit or conduits to which they are coupled. This may include heating the conduits to a temperature from about 25 °C to about 150 °C. In some other implementations, these temperature control apparatuses 951D-951H may be active coolers configured to actively cool respective conduit or conduits to which they are coupled. This may include actively cooling the conduits to a temperature from about 0 °C to about 25 °C. In some other implementations these temperature control apparatuses 951D-951H may be both heaters and active coolers, like described above. In some instances, these temperature control apparatuses 951D-951H may each be a heater and other temperature control apparatus 955D-955H that are each an active cooler may be coupled to each of the respective flowpaths thereby providing both active heating and cooling of the respective flowpaths.
[0129] The system 900 may also have one or more feedback control loops for controlling the temperature of the flowpaths using the temperature control apparatuses 951D-951H, the other temperature control apparatuses 955D-955H, or both, such as using PID or PLC control. This feedback control loop may have one or more controllers and temperature sensors, not depicted, coupled to one or more conduits of a respective flowpath, configured to detect the temperature of the conduit, or inside the conduit, and generate temperature sensor data indicative of that temperature. The one or more controllers are configured to receive the temperature data generated by the various temperature sensors and to control the temperature control apparatuses 951D-951H and 955D-955H in order to cause the temperature of the one or more conduits of the respective flowpaths to be at a particular temperature, or within a range of the particular temperature such as within about 1%, 5%, 10%, or 20%. This may include temperaturesDocket No. BLUCP027WOranging from about 0 °C to about 150 °C. For example, the first flowpath 316 may be actively heated by heater 951D and actively cooled by temperature control apparatus 955D, and controlled by a controller, such as by PID control, to one or more temperatures within the range of about 0 °C to about 150 °CExample Battery-Related Materials for Testing
[0130] Examples of materials used in battery manufacturing include graphite, silicon, carbon coated silicon, carbon structures embedded with silicon, silicon alloys (e.g., silicon alloyed with one or more of Al, Zn, Fe, Mn, Cr, Co, Ni, Cu, Ti, Mg, Sn, and Ge), silicon oxides (e.g. SiOx where 0 < x < 2), lithium titanium oxide, similar anode active materials or combinations thereof.
[0131] Examples of cathode active materials include lithium nickel manganese cobalt oxide (LiNixMnyCozCh) (“NMC”) where (x = 0.8, y = 0.1, z = 0.1; x = 0.6, y = 0.2, z = 0.2; x = 0.5, y = 0.3, z = 0.2; or x = 0.1, y = 0.1, z = 0.1), lithium nickel cobalt aluminum oxide (LiNixCoyAlzCE) (“NCA”) where (x = 0.80, y = 0.15, z = 0.05), lithium manganese oxide (LiMmCh) (“LMO”), lithium iron phosphate (LiFePCE) (“LFP”), lithium sulfide (Li2S), elemental sulfur (Ss), lithium cobalt oxide (LiCoCE), iron (II) fluoride (FeF2), iron (III) fluoride (FeFs), cobalt (II) fluoride (C0F2), similar cathode active materials or combinations thereof.
[0132] Both a cathode and anode may independently include a carbon additive to provide electrical conduction such as graphene, activated carbons, carbon fibers carbon black, Ketjen black, acetylene black, carbon nanotubes, graphite, C-ENERGY SUPER C65, C-ENERGY SUPER C45, SUPER P Li carbon black, or similar. In some embodiments, a conductive additive may be omitted. For example, a conductive additive may be omitted in some embodiments in which carbon-coated silicon or a silicon-carbon composite is used as the active material in the anode.
[0133] The electrodes may have a binder to provide electrode cohesion and adhesion strength. The binder is generally an organic polymer. Examples of binders include styrene butadiene rubber (SBR), styrene-isoprene-styrene (SIS), styrene-ethylene-butylene-styrene (SEBS), carboxymethyl cellulose (CMC), poly-acrylic acid (PAA), nitrile rubber (NBR), fluorinated block copolymers such as polyvinylidene fluoride (PVDF), or similar block copolymers. Further examples of polymers are provided below in the discussion of the separator. According to various embodiments, the polymer may or may not be an ionic conductor. Examples of polymers that are ionically conductive include polyethylene oxide) (PEG) and PEO-based block copolymers having lithium salts dissolved in them.Docket No. BLUCP027WO
[0134] Each of the anode and cathode electrolyte may be an inorganic electrolyte. It may be an oxide-based composition, a sulfide-based composition, or a phosphate-based composition, and may be crystalline, partially crystalline, or amorphous. In certain embodiments, the inorganic phase may be doped to increase conductivity. Examples of solid lithium ion conducting materials include perovskites (e.g., Li3xLa(2 / 3)- TiO3, 0 < x <.67), lithium super ionic conductor (LISICON) compounds (e.g., Li2+2xZm-xGeO4, 0 < x < 1; Lii4ZnGe40ie), thio-LISICON compounds (e.g., Li4-xAi-yByS4, A is Si, Ge or Sn, B is P, Al, Zn, Ga; LiioSnP2Si2), garnets (e.g. LivLasZ O^, LisLasAhOn, M is Ta or Nb); NASICON-type Li ion conductors (e.g., Lii.3Alo.3Tii.7(P04)3), oxide glasses or glass ceramics (e.g., Li3BO3-Li2SO4, Li2O-P2O5, Li2O-SiO2), argyrodites (e.g. LiePSsX where X = Cl, Br, I), sulfide glasses or glass ceramics (e.g., 75Li2S-25P2S5, Li2S-SiS2, LiI-Li2S-B2S3) and phosphates (e.g., Lii-xAlxGe2- (PO4)3 (LAGP), Lii+xTi2-xAlx(PO4)). Further examples include lithium rich anti-perovskite (LiRAP) particles. As described in Zhao and Daement, Jour J. Am. Chem. Soc., 2012, 134 (36), pp 15042-15047, incorporated by reference herein, these LiRAP particles have an ionic conductivity of greater than 10’3S / cm at room temperature.
[0135] Examples of solid lithium ion conducting materials include sodium super ionic conductor (NASICON) compounds (e.g., Nai+xZr2SixP3- Oi2, 0 < x < 3). Further examples of solid lithium ion conducting materials may be found in Cao et al., Front. Energy Res. (2014) 2:25 and Knauth, Solid-state Ionics 180 (2009) 911-916, both of which are incorporated by reference herein.
[0136] Further examples of ion conducting glasses are disclosed in Ribes et al., J. Non-Cryst. Solids, Vol. 38-39 (1980) 271-276 and Minami, J. Non-Cryst. Solids, Vol. 95-96 (1987) 107-118, which are incorporated by reference herein.
[0137] In some embodiments, the solid electrolytes are argyrodites. The argyrodites may have the general formula: Av-xPSe- Halx where A is an alkali metal and Hal is selected from chlorine (Cl), bromine (Br), and iodine (I).
[0138] In some embodiments, the argyrodite may have a general formula as given above, and further be doped. An example is argyrodites doped with thiophilic metals:A7-x-(z*m)MzmPS6- Halx wherein A is an alkali metal; M is a metal selected from manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni), copper (Cu), zinc (Zn), and mercury (Hg); Hal is selected from chlorine (Cl), bromine (Br), and iodine (I); z is the oxidation state of the metal; 0 < x < 2; and 0 < y < (7-x) / z. In some embodiments, A is lithium (Li), sodium (Na) or potassium (K). In some embodiments, A is Li. Metal-doped argyrodites are described further in U. S. Patent Application No. 16 / 829,962, incorporated by reference herein. In someDocket No. BLUCP027WOembodiments, the composite may include oxide argyrodites, for example, as described in U. S. Patent Application No. 16 / 576,570, incorporated by reference herein.
[0139] Alkali metal argyrodites more generally are any of the class of conductive crystals of cubic symmetry that include an alkali metal. This includes argyrodites of the formulae given above as well as argyrodites described in US Patent Publication No. 20170352916 which include Liy-x+yPSe-xClx+y where x and y satisfy the formula 0.05<y<0.9 and -3.0x+1.8<y<- 3.0x+5, or other argyrodites with Ay- +yPSe- Hal +y formula. Such argyrodites may also be doped with metal as described above, which include A7- +y-(z*m)MzmPS6- Hal +y.
[0140] In some embodiments, the active material particles may first be coated by solid electrolyte prior to mixing a slurry, to improve contact between the active material and solid electrolyte.
[0141] For cathode compositions, the table below gives examples of compositions.ElectronicActive InorganicConstituent conductivity Organic phase material conductoradditiveExamples • Transition • Argyrodites • Carbon• Hydrophobic block j Metal Oxide (e.g., LiePSsCl, based copolymers having | • NCA Li5.6PS4.6C11.4, • Activated soft and hard blocks j • NMC Li5.4Mo.lPS4.6C11.4 carbons • PVDF and SEBS i • LFP, Lis.sMo.iPSsCl, • CNTs • PMMA and SEBS i • Sulfur Nas.sMo.iPSsCl • Graphene • Nylon and SEBS • Sulfide glasses • Graphite • SEBSor glass ceramics • Carbon • SIS(e.g., fibers • PMMA75Li2S-25P2S5) • Carbon • PVDF• LiioGeP2Si2black (e.g., • PS-PVDF (LGPS) Super C) • PVDF grafted with PS• NBR• Grafted SEBS with polar polymer blocks10% -33% l%-5% l%-5%Docket No. BLUCP027WO
[0142] For anode compositions, the table below gives examples of compositions.Primary Secondary ElectronicInorganicConstituent active active conductivity Organic phase conductormaterial material additiveExamples • Silicon • Graphite • Argyrodites • Carbon•Hydrophobic oxide (e.g., LiePSsCl, based block• Si-C Li5.6PS4.6C11.4, • Activated copolymers composites Li5.4M0.lPS4.6C carbons having soft • Elemental 11.4, • CNTs and hard Si Lis.sMo.iPSsCl, • Graphene blocks• Si alloys, Nas.sMo.iPSsCl • Carbon •PVDF and e.g., Si • Sulfide fibers SEBS alloyed with glasses or glass • Carbon •PMMA and one or more ceramics (e.g., black (e.g., SEBS of Al, Zn, Fe, 75Li2S-25P2S5) Super C) •Nylon and Mn, Cr, Co, • LiioGeP2Si2 SEBS Ni, Cu, Ti, (LGPS) •CMC and Mg, Sn, Ge PAA• Graphite •PAA• Sn •PVA• SEBS• SIS •NBR •PVDF •PS-PVDF •PVDF grafted with PS•Grafted SEBS with polar polymer blocks Wt % range Si is 15%- 5%-40% io%-6o% 0%-5% 1% 5%50%Additional and / or Alternative Embodiments
[0143] Unless otherwise specified, the illustrated embodiments are to be understood as providing example features of varying detail of some embodiments. Thus, unless otherwise specified, the features, components, modules, layers, films, regions, aspects, structures, etc. (hereinafter individually or collectively referred to as an “element” or “elements”), of the various illustrations may be otherwise combined, separated, interchanged, and / or rearranged without departing from the teachings of the disclosure.
[0144] The terminology used herein is for the purpose of describing some embodiments and is not intended to be limiting. As used herein, the singular forms, “a,” “an,” and “the” areDocket No. BLUCP027WOintended to include the plural forms as well, unless the context clearly indicates otherwise. It is to be understood that the phrases “for each <item> of the one or more <items>,” “each <item> of the one or more <items>,” and / or the like, if used herein, are inclusive of both a single-item group and multiple-item groups, i.e., the phrase “for... each” is used in the sense that it is used in programming languages to refer to each item of whatever population of items is referenced. For example, if the population of items referenced is a single item, then “each” would refer to only that single item (despite dictionary definitions of “each” frequently defining the term to refer to “every one of two or more things”) and would not imply that there must be at least two of those items. Similarly, the term “set” or “subset” should not be viewed, in itself, as necessarily encompassing a plurality of items — it is to be understood that a set or a subset can encompass only one member or multiple members (unless the context indicates otherwise). The terms “comprises,” “comprising,” “includes,” and / or “including,” when used in this specification, specify the presence of stated features, integers, steps, operations, elements, components, and / or groups thereof, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and / or groups thereof. It is also noted that, as used herein, the terms “substantially,” “about,” and other similar terms, are used as terms of approximation and not as terms of degree, and, as such, are utilized to account for inherent deviations in measured, calculated, and / or provided values that would be recognized by one of ordinary skill in the art. Accordingly, the term “substantially” as used herein, unless otherwise specified, means within 5% of a referenced value. For example, substantially perpendicular means within ±5% of parallel.
[0145] The use of cross-hatching and / or shading in the accompanying drawings is generally provided to clarify boundaries between adjacent elements. As such, neither the presence nor the absence of cross-hatching or shading conveys or indicates any preference or requirement for particular materials, material properties, dimensions, proportions, commonalities between illustrated elements, and / or any other characteristic, attribute, property, etc., of the elements, unless specified. Further, in the accompanying drawings, the size and relative sizes of elements may be exaggerated for clarity and / or descriptive purposes. As such, the sizes and relative sizes of the respective elements are not necessarily limited to the sizes and relative sizes shown in the drawings. When an embodiment may be implemented differently, a specific process order may be performed differently from the described order. For example, two consecutively described processes may be performed substantially at the same time or performed in an order opposite to the described order.Docket No. BLUCP027WO
[0146] When an element, such as a layer, is referred to as being “on,” “connected to,” or “coupled to” another element, it may be directly on, directly connected to, or directly coupled to the other element or at least one intervening element may be present. When, however, an element is referred to as being “directly on,” “directly connected to,” or “directly coupled to” another element, there are no intervening elements present. Other terms and / or phrases if used herein to describe a relationship between elements should be interpreted in a like fashion, such as “between” versus “directly between,” “adjacent” versus “directly adjacent,” “on” versus “directly on,” etc. Further, the term “connected” may refer to physical, electrical, and / or fluid connection. To this end, for the purposes of this disclosure, the phrase “fluidically connected” is used with respect to volumes, plenums, holes, etc., that may be connected to one another, either directly or via one or more intervening components or volumes, to form a fluidic connection, similar to how the phrase “electrically connected” is used with respect to components that are connected to form an electric connection. The phrase “fluidically interposed,” if used, may be used to refer to a component, volume, plenum, hole, etc., that is fluidically connected with at least two other components, volumes, plenums, holes, etc., such that fluid flowing from one of those other components, volumes, plenums, holes etc., to the other or another of those components, volumes, plenums, holes, etc., would first flow through the “fluidically interposed” component before reaching that other or another of those components, volumes, plenums, holes, etc.. For example, if a pump is fluidically interposed between a reservoir and an outlet, fluid flowing from the reservoir to the outlet would first flow through the pump before reaching the outlet. The phrase "fluidically adjacent," if used, refers to placement of a fluidic element relative to another fluidic element such that no potential structures fluidically are interposed between the two elements that might potentially interrupt fluid flow between the two fluidic elements. For example, in a flow path having a first valve, a second valve, and a third valve arranged sequentially there along, the first valve would be fluidically adjacent to the second valve, the second valve fluidically adjacent to both the first and third valves, and the third valve fluidically adjacent to the second valve.
[0147] For the purposes of this disclosure, “at least one of X, Y,..., and Z” and “at least one selected from the group consisting of X, Y,..., and Z” may be construed as X only, Y only,..., Z only, or any combination of two or more of X, Y,..., and Z, such as, for instance, XYZ, XYY, YZ, and ZZ. As used herein, the term “and / or” includes any and all combinations of one or more of the associated listed items.
[0148] Although the terms “first,” “second,” “third,” etc., may be used herein to describe various elements, these elements should not be limited by these terms. These terms are usedDocket No. BLUCP027WOto distinguish one element from another element. Thus, a first element discussed below could be termed a second element without departing from the teachings of the disclosure. To this end, use of such identifiers, e.g., “a first element,” should not be read as suggesting, implicitly or inherently, that there is necessarily another instance, e.g., “a second element.” Further, the use, if any, of ordinal indicators, such as (a), (b), (c),..., or (1), (2), (3),..., or the like, in this disclosure and accompanying claims, is to be understood as not conveying any particular order or sequence, except to the extent that such an order or sequence is explicitly indicated. For example, if there are three steps labeled (i), (ii), and (iii), it is to be understood that these steps may be performed in any order (or even concurrently, if not otherwise contraindicated), unless indicated otherwise. For example, if step (ii) involves the handling of an element that is created in step (i), then step (ii) may be viewed as happening at some point after step (i). In a similar manner, if step (i) involves the handling of an element that is created in step (ii), the reverse is to be understood.
[0149] Spatially relative terms, such as “beneath,” “below,” “under,” “lower,” “above,” “upper,” “over,” “higher,” “side” (e.g., as in “sidewall”), and the like, may be used herein for descriptive purposes, and, thereby, to describe one element’s spatial relationship to at least one other element as illustrated in the drawings. Spatially relative terms are intended to encompass different orientations of an apparatus in use, operation, and / or manufacture in addition to the orientation depicted in the drawings. For example, if the apparatus in the drawings is turned over, elements described as “below” or “beneath” other elements or features would then be oriented “above” or “over” the other elements or features. Thus, the term “below” can encompass both an orientation of above and below. Furthermore, the apparatus may be otherwise oriented (e.g., rotated 90 degrees or at other orientations), and, as such, the spatially relative descriptors used herein interpreted accordingly.
[0150] The term “between,” as used herein and when used with a range of values, is to be understood, unless otherwise indicated, as being inclusive of the start and end values of that range. For example, between 1 and 5 is to be understood as inclusive of the numbers 1, 2, 3, 4, and 5, not just the numbers 2, 3, and 4.
[0151] As used herein, the phrase “operatively connected” is to be understood as referring to a state in which two components and / or systems are connected, either directly or indirectly, such that, for example, at least one component or system can control the other. For instance, a controller may be described as being operatively connected with (or to) a resistive heating unit, which is inclusive of the controller being connected with a sub-controller of the resistive heating unit that is electrically connected with a relay that is configured to controllably connectDocket No. BLUCP027WOor disconnect the resistive heating unit with a power source that is capable of providing an amount of power that is able to power the resistive heating unit so as to generate a desired degree of heating. The controller itself likely will not supply such power directly to the resistive heating unit due to the current(s) involved, but it is to be understood that the controller is nonetheless operatively connected with the resistive heating unit.
[0152] As used herein, the singular forms, “a,” “an,” and “the” are intended to include the plural forms as well, unless the context clearly indicates otherwise. It is also to be understood that the phrases “for each <item> of the one or more <items>,” “each <item> of the one or more <items>,” and / or the like, if used herein, are inclusive of both a single-item group and multiple-item groups, i.e., the phrase “for... each” is used in the sense that it is used in programming languages to refer to each item of whatever population of items is referenced. For example, if the population of items referenced is a single item, then “each” would refer to only that single item (despite dictionary definitions of “each” frequently defining the term to refer to “every one of two or more things”) and would not imply that there must be at least two of those items. Similarly, the term “set” or “subset” should not be viewed, in itself, as necessarily encompassing a plurality of items — it is to be understood that a set or a subset can encompass only one member or multiple members (unless the context indicates otherwise). In addition, the terms “comprises,” “comprising,” “includes,” and / or “including,” when used in this specification, specify the presence of stated features, integers, steps, operations, elements, components, and / or groups thereof, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and / or groups thereof.
[0153] Various embodiments are described herein with reference to sectional views, isometric views, perspective views, plan views, and / or exploded illustrations that are schematic depictions of idealized embodiments and / or intermediate structures. As such, variations from the shapes of the illustrations as a result of, for example, manufacturing techniques and / or tolerances, are to be expected. Thus, embodiments disclosed herein should not be construed as limited to the particular illustrated shapes of regions, but are to include deviations in shapes that result from, for instance, manufacturing. To this end, regions illustrated in the drawings may be schematic in nature and shapes of these regions may not reflect the actual shapes of regions of a device, and, as such, are not intended to be limiting.
[0154] Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure is a part. Terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the contextDocket No. BLUCP027WOof the relevant art and are not to be interpreted in an idealized or overly formal sense, unless expressly so defined herein.
[0155] As customary in the field, some embodiments are described and illustrated in the accompanying drawings in terms of functional blocks, units, and / or modules. Those skilled in the art will appreciate that these blocks, units, and / or modules are physically implemented by electronic (or optical) circuits, such as logic circuits, discrete components, microprocessors, hard-wired circuits, memory elements, wiring connections, and the like, which may be formed using semiconductor-based fabrication techniques or other manufacturing technologies. In the case of the blocks, units, and / or modules being implemented by microprocessors or other similar hardware, they may be programmed and controlled using software (e.g., microcode) to perform various functions discussed herein and may optionally be driven by firmware and / or software. It is also contemplated that each block, unit, and / or module may be implemented by dedicated hardware, or as a combination of dedicated hardware to perform some functions and a processor (e.g., one or more programmed microprocessors and associated circuitry) to perform other functions. Also, each block, unit, and / or module of some embodiments may be physically separated into two or more interacting and discrete blocks, units, and / or modules without departing from the inventive concepts. Further, the blocks, units, and / or modules of some embodiments may be physically combined into more complex blocks, units, and / or modules without departing from the teachings of the disclosure.
[0156] Although the foregoing embodiments have been described in some detail for purposes of clarity of understanding, it will be apparent that certain changes and modifications may be practiced within the scope of the appended claims. It should be noted that there are many alternative ways of implementing the processes, systems, and apparatuses of the disclosed embodiments. Accordingly, embodiments are to be considered as illustrative and not as restrictive, and embodiments are not to be limited to the details given herein.
[0157] It is to be understood that the above disclosure, while focusing on a particular example implementation or implementations, is not limited to only the discussed example, but may also apply to similar variants and mechanisms as well, and such similar variants and mechanisms are also considered to be within the scope of this disclosure. For example, the above disclosure is directed to at least, but not exclusively, the following numbered implementations.
[0158] Implementation 1. A sample testing system, comprising: a mixing chamber having a first inlet, a second inlet, and an outlet; a first source of a first gas fluidically connected to the first inlet of the mixing chamber via a first flowpath, wherein the first gas and a first component flow from the first flowpath to the mixing chamber; a first mass flow controller (MFC)Docket No. BLUCP027WOfluidically interposed along the first flowpath and configured to control the flow of the first gas to the mixing chamber; a second source of second gas fluidically connected to the second inlet of the mixing chamber via a second flowpath; a second MFC fluidically interposed along the second flowpath and configured to control the flow of the second gas to the mixing chamber; a sample chamber having a sample chamber inlet fluidically connected to the outlet of the mixing chamber by a first outlet flowpath; a first sensor configured to detect the first component inside the mixing chamber and generate data indicative of a first concentration of the first component in the mixing chamber; and a first controller communicatively connected to the first sensor and the first MFC, and configured to: receive first sensor data from the first sensor, and control, based at least in part on the first sensor data, the first MFC to control a flowrate of the first gas through the first MFC and thereby cause a first desired concentration of the first component to be in the mixing chamber, wherein a testing mixture comprising the first gas, the dry air, and the first component is configured to flow from the mixing chamber to the sample chamber inlet through the first outlet flowpath.
[0159] Implementation 2. The system of implementation 1, further comprising: a sensor chamber fluidically connected to a sample chamber outlet of the sample chamber by a second outlet flowpath spanning from the sample chamber outlet to the sensor chamber such that gas is configured to flow from the sample chamber to the sensor chamber through the second outlet flowpath; and a second sensor coupled to the sensor chamber and configured to detect a second component in the sensor chamber and generate second sensor data indicative of a second amount of the second component in the sensor chamber.
[0160] Implementation 3. The system of implementation 2, further comprising a third sensor coupled to the sensor chamber and configured to detect the second component in the sensor chamber and generate third sensor data indicative of a third amount of the second component in the sensor chamber.
[0161] Implementation 4. The system of implementation 2, wherein the second component comprises water, sulfur dioxide, sulfur vapor, oxygen, hydrogen, hydrogen sulfide, carbon dioxide, carbon monoxide.
[0162] Implementation 5. The system of implementation 2, further comprising a fourth sensor coupled to the sensor chamber and configured to detect the first component in the sensor chamber and generate fourth sensor data indicative of a fourth amount of the first component in the sensor chamber.
[0163] Implementation 6. The system of implementation 2, further comprising: a first valve having a first valve inlet, a first valve outlet, and a second valve outlet, and fluidicallyDocket No. BLUCP027WOinterposed along the first outlet flowpath; a second valve having a second valve inlet, a third valve inlet, and a third valve outlet, and fluidically interposed along the second outlet flowpath; and a bypass flowpath spanning from, and fluidically connecting, the second valve outlet of the first valve to the third valve inlet of the second valve, wherein: the sample chamber inlet is fluidically connected to the first valve outlet of the first valve, the sample chamber outlet is fluidically connected by the second outlet flowpath to the second valve inlet of the second valve, in a first configuration, the first valve is configured to cause the testing mixture flowing through the first valve inlet to flow out the first valve outlet to the sample chamber, in a second configuration, the first valve is configured to cause the testing mixture flowing through the first valve inlet to flow out the second valve outlet to the bypass flowpath, in a third configuration, the second valve is configured to cause gas flowing from the sample chamber through the third valve inlet to flow out the third valve outlet to the sensor chamber, and in a fourth configuration, the second valve is configured to cause gas flowing from the bypass flowpath through the third valve inlet to flow out the third valve outlet to the sensor chamber.
[0164] Implementation 7. The system of implementation 6, wherein when the first valve is in the first configuration and the second valve is in the third configuration, the testing mixture is caused to flow from the mixing chamber to the sample chamber, and gas comprising the testing mixture is caused to flow from the sample chamber to the sensor chamber.
[0165] Implementation 8. The system of implementation 6, further comprising: an exhaust flowpath fluidically connected to the bypass flowpath; and an exhaust valve fluidically interposed along the exhaust flowpath and configured to control flow of gas through the exhaust flowpath, wherein gas flowing in the bypass flowpath is configured to flow to and through the exhaust flowpath when the exhaust valve is in an open position.
[0166] Implementation 9. The system of implementation 6, further comprising: a third valve having a fourth valve inlet, a fifth valve inlet, and a fourth valve outlet, and fluidically interposed along the first outlet flowpath and fluidically interposed between the first valve and the sample chamber; and an inert gas source fluidically connected to the fifth valve inlet of the third valve and configured to flow the inert gas into the sample chamber, wherein: in a fifth configuration, the third valve is configured to cause gas flowing through the fourth valve inlet to flow out the fourth valve outlet and to the sample chamber, and in a sixth configuration, the third valve is configured to cause the inert gas flowing through the fifth valve inlet to flow out the fourth valve outlet and to the sample chamber.Docket No. BLUCP027WO
[0167] Implementation 10. The system of implementation 6, further comprising a pressure relief valve fluidically interposed along the first outlet flowpath and interposed between the first valve and the mixing chamber.
[0168] Implementation 11. The system of implementation 6, further comprising a second controller configured to control operation of the first valve and the second valve, and having one or more processors and one or more memories storing instructions for causing the one or more processors to cause: the first valve to be in the first configuration and the second valve to be in the fourth configuration at the same time and thereby causing the testing mixture to flow from the mixing chamber to the sample chamber, and causing gas comprising the testing mixture to flow from the sample chamber to the sensor chamber, and the first valve to be in the second configuration and the second valve to be in the third configuration at the same time and thereby causing the testing mixture to flow from the mixing chamber to the bypass flowpath and not to sample chamber.
[0169] Implementation 12. The system of implementation 1, further comprising a liquid source fluidically interposed along the first flowpath, wherein: the liquid comprises the first component, and the first gas is configured to receive the first component from the liquid source and form a first mixture comprising the first gas and the first component.
[0170] Implementation 13. The system of implementation 12, wherein the liquid source is water and the first component is water.
[0171] Implementation 14. The system of implementation 12, wherein the first component is a vapor in the first gas.
[0172] Implementation 15. The system of implementation 12, wherein the first gas is dry air.
[0173] Implementation 16. The system of implementation 1, wherein the second gas is dry air.
[0174] Implementation 17. The system of implementation 1, wherein the dry air comprises less than 25% oxygen, less than 5% hydrogen, less than 3% carbon dioxide, less than 3% carbon monoxide, and greater than 70% nitrogen.
[0175] Implementation 18. The system of implementation 1, further comprising: a first valve having a first valve inlet, a first valve outlet, and a second valve outlet, and fluidically interposed along the first outlet flowpath; and a bypass flowpath spanning from the second valve outlet to an exhaust, wherein: the sample chamber inlet is fluidically connected to the first valve outlet, in a first configuration, the first valve is configured to cause the testing mixture flowing through the first valve inlet to flow out the first valve outlet, and in a second configuration, the first valve is configured to cause the testing mixture flowing through the first valve inlet to flow out the second valve outlet.Docket No. BLUCP027WO
[0176] Implementation 19. The system of implementation 18, wherein the first valve outlet and the second valve outlet are oriented with respect to each other at less than 180 degrees.
[0177] Implementation 20. The system of implementation 1, further comprising an inert gas source fluidically connected to the sample chamber and configured to flow the inert gas into the sample chamber.
[0178] Implementation 21. The system of implementation 1, wherein the first controller is a proportional integral derivative (PID) controller.
[0179] Implementation 22. The system of implementation 1, wherein the sample chamber: has a chamber interior, an interior inlet configured to flow gas from the sample chamber inlet into the chamber interior, and an interior outlet configured to flow gas out of the chamber interior to a sample chamber outlet, is configured to support a sample in the chamber interior at a first offset distance from the interior inlet, and is configured to support the sample in the chamber interior at a second offset distance, less than the first offset distance, from the interior inlet.
[0180] Implementation 23. The system of implementation 22, wherein: at the first offset distance, the sample chamber is configured to cause gas flowing into the chamber interior to be turbulent flow, and at the second offset distance, the sample chamber is configured to cause gas flowing into the chamber interior to be diffuse flow.
[0181] Implementation 24. The system of implementation 1, further comprising: a third source of a third gas fluidically connected to a third inlet of the mixing chamber via a third flowpath, wherein the third gas and a third component flow from the third flowpath to the mixing chamber; a third MFC fluidically interposed along the third flowpath and configured to control the flow of the third gas to the mixing chamber; a fifth sensor configured to detect the third component inside the mixing chamber and generate fifth sensor data indicative of a fifth concentration of the third component in the mixing chamber; and a third controller communicatively connected to the fifth sensor and the third MFC, and configured to: receive third sensor data from the fifth sensor, and control, based at least in part on the fifth sensor data, the third MFC to control a flowrate of the third gas through the third MFC and thereby cause a third desired concentration of the third component to be in the mixing chamber, wherein the testing mixture comprising the first gas, the second gas, the first component, the third gas, and the third component is configured to flow from the mixing chamber to the sample chamber inlet through the first outlet flowpath.
[0182] Implementation 25. The system of implementation 1, further comprising one or more temperature control apparatuses coupled to one or more of the mixing chamber, the sample chamber, one or more conduits of the first flowpath, one or more conduits of the secondDocket No. BLUCP027WOflowpath, or one or more conduits of the outlet flowpath, wherein: each temperature control apparatus is configured to control a temperature of the mixing chamber, the sample chamber, one or more conduits of the first flowpath, one or more conduits of the second flowpath, one or more conduits of the outlet flowpath to which it is coupled, and the temperature ranges from about 0 °C to about 150 °C.
[0183] Implementation 26. The system of implementation 25, wherein at least one temperature control apparatus is a heater, an active cooler, or both.
[0184] Implementation 27. The system of implementation 25, further comprising one or more second temperature control apparatuses coupled to one or more of the mixing chamber, the sample chamber, one or more conduits of the first flowpath, one or more conduits of the second flowpath, or one or more conduits of the outlet flowpath, wherein: each second temperature control apparatus is configured to control a second temperature of the mixing chamber, the sample chamber, one or more conduits of the first flowpath, one or more conduits of the second flowpath, or one or more conduits of the outlet flowpath to which it is coupled, the temperature ranges from about 25 °C to about 150 °C, and the second temperature ranges from about 0 °C to about 25 °C.
[0185] Implementation 28. The system of implementation 1, wherein: the first inlet and the second inlet are positioned at a bottom portion of the mixing chamber, and the first inlet is oriented at a non-parallel angle with respect to the second inlet.
[0186] Implementation 29. A method for sample testing, the method comprising: flowing, by a first mass flow controller (MFC), a first gas and a first component through a first flowpath to a first inlet of a mixing chamber; flowing, by a second MFC, a second gas through a second flowpath to a second inlet of the mixing chamber; generating first sensor data, using a first sensor configured to detect the first component inside the mixing chamber, indicative of a first concentration of the first component in the mixing chamber; controlling, based at least in part on the first sensor data, the first MFC to control the flow of first gas and the first component and thereby causing a first desired concentration of the first component to be in the mixing chamber; and flowing a testing mixture comprising the first gas, the second gas, and the first component from the mixing chamber to a sample chamber through a first outlet flowpath fluidically connecting the mixing chamber and the sample chamber.
[0187] Implementation 30. The method of implementation 29, further comprising: flowing gas from the sample chamber to a sensor chamber through a second outlet flowpath, wherein a second sensor is coupled to the sensor chamber and configured to detect a second component in the sensor chamber and generate second sensor data indicative of a second amount of theDocket No. BLUCP027WOsecond component in the sensor chamber; and generating the second sensor data, by the second sensor, indicative of the second amount of the second component in the sensor chamber.
[0188] Implementation 31. The method of implementation 30, wherein: the first outlet flowpath further comprises a first valve having a first valve inlet, a first valve outlet, and a second valve outlet, wherein a sample chamber inlet is fluidically connected to the first valve outlet, the second outlet flowpath further comprises a second valve having a second valve inlet, a third valve inlet, and a third valve outlet, wherein a sample chamber outlet is fluidically connected by the second outlet flowpath to the third valve inlet of the second valve, a bypass flowpath spans from, and fluidically connects, the second valve outlet of the first valve to the second valve inlet of the second valve, and the method further comprises: flowing the testing mixture to the sample chamber and the sensor chamber, and not the bypass flowpath, by positioning the first valve in a first configuration and thereby causing the testing mixture to flow through the first valve inlet and flow out the first valve outlet to the sample chamber, and by positioning the second valve in a third configuration and thereby causing the gas flowing from the sample chamber to flow through the third valve inlet to flow out the third valve outlet to the sensor chamber; and flowing the testing mixture to the bypass flowpath and the sensor chamber, and not to the sample chamber, by positioning the first valve in a second configuration and thereby causing the testing mixture to flow through the first valve inlet to flow out the second valve outlet to the bypass flowpath, and by positioning the second valve in a fourth configuration and thereby causing gas flowing in the bypass flowpath to flow through the third valve inlet to flow out the third valve outlet to the sensor chamber.
[0189] Implementation 32. The method of implementation 31, further comprising changing the flow of the testing mixture from flowing through the bypass flowpath to flowing through the sample chamber by changing the second valve from the third configuration to the fourth configuration and changing the first valve from the second configuration to the first configuration.
[0190] Implementation 33. The method of implementation 32, further comprising opening, before or during changing the flow of the testing mixture from flowing through the bypass flowpath to flowing through the sample chamber, an exhaust valve fluidically connected to an exhaust flowpath fluidically connected to the bypass flowpath and thereby causing the testing mixture to flow from the bypass flowpath to the exhaust flowpath.
[0191] Implementation 34. The method of implementation 32, wherein changing the second valve from the third configuration to the fourth configuration occurs at the same time, or before, changing the first valve from the second configuration to the first configuration.Docket No. BLUCP027WO
[0192] Implementation 35. The method of implementation 31, further comprising changing the flow of the testing mixture from flowing through the bypass flowpath to flowing through the bypass flowpath by changing the second valve from the fourth configuration to the third configuration and changing the first valve from the first configuration to the second configuration.
[0193] Implementation 36. The method of implementation 30, further comprising generating, by a third sensor coupled to the sensor chamber and configured to detect the first component in the sensor chamber, third sensor data indicative of the first component in the sensor chamber.
[0194] Implementation 37. The method of implementation 29, further comprising: flowing, by a third MFC, a third gas and a third component through a third flowpath to a third inlet of the mixing chamber; generating fifth sensor data, using a fifth sensor configured to detect the third component inside the mixing chamber, indicative of a third concentration of the third component in the mixing chamber; controlling, based at least in part on the fifth sensor data, the third MFC to control the flow of third gas and the third component and thereby causing a third desired concentration of the third component to be in the mixing chamber; and the flowing the testing mixture further comprises flowing the first gas, the second gas, the first component, the third gas, and the third component from the mixing chamber to the sample chamber through the first outlet flowpath.
Claims
Docket No. BLUCP027WOCLAIMSWhat is claimed is:
1. A sample testing system, comprising:a mixing chamber having a first inlet, a second inlet, and an outlet;a first source of a first gas fluidically connected to the first inlet of the mixing chamber via a first flowpath, wherein the first gas and a first component flow from the first flowpath to the mixing chamber;a first mass flow controller (MFC) fluidically interposed along the first flowpath and configured to control the flow of the first gas to the mixing chamber;a second source of second gas fluidically connected to the second inlet of the mixing chamber via a second flowpath;a second MFC fluidically interposed along the second flowpath and configured to control the flow of the second gas to the mixing chamber;a sample chamber having a sample chamber inlet fluidically connected to the outlet of the mixing chamber by a first outlet flowpath;a first sensor configured to detect the first component inside the mixing chamber and generate data indicative of a first concentration of the first component in the mixing chamber; anda first controller communicatively connected to the first sensor and the first MFC, and configured to:receive first sensor data from the first sensor, andcontrol, based at least in part on the first sensor data, the first MFC to control a flowrate of the first gas through the first MFC and thereby cause a first desired concentration of the first component to be in the mixing chamber, wherein a testing mixture comprising the first gas, the dry air, and the first component is configured to flow from the mixing chamber to the sample chamber inlet through the first outlet flowpath.
2. The system of claim 1, further comprising:a sensor chamber fluidically connected to a sample chamber outlet of the sample chamber by a second outlet flowpath spanning from the sample chamber outlet to the sensor chamber such that gas is configured to flow from the sample chamber to the sensor chamber through the second outlet flowpath; andDocket No. BLUCP027WOa second sensor coupled to the sensor chamber and configured to detect a second component in the sensor chamber and generate second sensor data indicative of a second amount of the second component in the sensor chamber.
3. The system of claim 2, further comprising a third sensor coupled to the sensor chamber and configured to detect the second component in the sensor chamber and generate third sensor data indicative of a third amount of the second component in the sensor chamber.
4. The system of claim 2, further comprising a fourth sensor coupled to the sensor chamber and configured to detect the first component in the sensor chamber and generate fourth sensor data indicative of a fourth amount of the first component in the sensor chamber.
5. The system of claim 2, further comprising:a first valve having a first valve inlet, a first valve outlet, and a second valve outlet, and fluidically interposed along the first outlet flowpath;a second valve having a second valve inlet, a third valve inlet, and a third valve outlet, and fluidically interposed along the second outlet flowpath; anda bypass flowpath spanning from, and fluidically connecting, the second valve outlet of the first valve to the third valve inlet of the second valve, wherein:the sample chamber inlet is fluidically connected to the first valve outlet of the first valve,the sample chamber outlet is fluidically connected by the second outlet flowpath to the second valve inlet of the second valve,in a first configuration, the first valve is configured to cause the testing mixture flowing through the first valve inlet to flow out the first valve outlet to the sample chamber,in a second configuration, the first valve is configured to cause the testing mixture flowing through the first valve inlet to flow out the second valve outlet to the bypass flowpath, in a third configuration, the second valve is configured to cause gas flowing from the sample chamber through the third valve inlet to flow out the third valve outlet to the sensor chamber, andin a fourth configuration, the second valve is configured to cause gas flowing from the bypass flowpath through the third valve inlet to flow out the third valve outlet to the sensor chamber.Docket No. BLUCP027WO6. The system of claim 5, wherein when the first valve is in the first configuration and the second valve is in the third configuration, the testing mixture is caused to flow from the mixing chamber to the sample chamber, and gas comprising the testing mixture is caused to flow from the sample chamber to the sensor chamber.
7. The system of claim 5, further comprising:an exhaust flowpath fluidically connected to the bypass flowpath; andan exhaust valve fluidically interposed along the exhaust flowpath and configured to control flow of gas through the exhaust flowpath, wherein gas flowing in the bypass flowpath is configured to flow to and through the exhaust flowpath when the exhaust valve is in an open position.
8. The system of claim 5, further comprising:a third valve having a fourth valve inlet, a fifth valve inlet, and a fourth valve outlet, and fluidically interposed along the first outlet flowpath and fluidically interposed between the first valve and the sample chamber; andan inert gas source fluidically connected to the fifth valve inlet of the third valve and configured to flow the inert gas into the sample chamber, wherein:in a fifth configuration, the third valve is configured to cause gas flowing through the fourth valve inlet to flow out the fourth valve outlet and to the sample chamber, andin a sixth configuration, the third valve is configured to cause the inert gas flowing through the fifth valve inlet to flow out the fourth valve outlet and to the sample chamber.
9. The system of claim 5, further comprising a pressure relief valve fluidically interposed along the first outlet flowpath and interposed between the first valve and the mixing chamber.
10. The system of claim 5, further comprising a second controller configured to control operation of the first valve and the second valve, and having one or more processors and one or more memories storing instructions for causing the one or more processors to cause:the first valve to be in the first configuration and the second valve to be in the fourth configuration at the same time and thereby causing the testing mixture to flow from the mixing chamber to the sample chamber, and causing gas comprising the testing mixture to flow from the sample chamber to the sensor chamber, andDocket No. BLUCP027WOthe first valve to be in the second configuration and the second valve to be in the third configuration at the same time and thereby causing the testing mixture to flow from the mixing chamber to the bypass flowpath and not to sample chamber.
11. The system of claim 1, further comprising a liquid source fluidically interposed along the first flowpath, wherein:the liquid comprises the first component, andthe first gas is configured to receive the first component from the liquid source and form a first mixture comprising the first gas and the first component.
12. The system of claim 1, wherein the dry air comprises less than 25% oxygen, less than 5% hydrogen, less than 3% carbon dioxide, less than 3% carbon monoxide, and greater than 70% nitrogen.
13. The system of claim 1, further comprising:a first valve having a first valve inlet, a first valve outlet, and a second valve outlet, and fluidically interposed along the first outlet flowpath; anda bypass flowpath spanning from the second valve outlet to an exhaust, wherein: the sample chamber inlet is fluidically connected to the first valve outlet,in a first configuration, the first valve is configured to cause the testing mixture flowing through the first valve inlet to flow out the first valve outlet, andin a second configuration, the first valve is configured to cause the testing mixture flowing through the first valve inlet to flow out the second valve outlet.
14. The system of claim 1, wherein the sample chamber:has a chamber interior, an interior inlet configured to flow gas from the sample chamber inlet into the chamber interior, and an interior outlet configured to flow gas out of the chamber interior to a sample chamber outlet,is configured to support a sample in the chamber interior at a first offset distance from the interior inlet, andis configured to support the sample in the chamber interior at a second offset distance, less than the first offset distance, from the interior inlet.Docket No. BLUCP027WO15. The system of claim 14, wherein:at the first offset distance, the sample chamber is configured to cause gas flowing into the chamber interior to be turbulent flow, andat the second offset distance, the sample chamber is configured to cause gas flowing into the chamber interior to be diffuse flow.
16. The system of claim 1, further comprising one or more temperature control apparatuses coupled to one or more of the mixing chamber, the sample chamber, one or more conduits of the first flowpath, one or more conduits of the second flowpath, or one or more conduits of the outlet flowpath, wherein:each temperature control apparatus is configured to control a temperature of the mixing chamber, the sample chamber, one or more conduits of the first flowpath, one or more conduits of the second flowpath, one or more conduits of the outlet flowpath to which it is coupled, and the temperature ranges from about 0 °C to about 150 °C.
17. A method for sample testing, the method comprising:flowing, by a first mass flow controller (MFC), a first gas and a first component through a first flowpath to a first inlet of a mixing chamber;flowing, by a second MFC, a second gas through a second flowpath to a second inlet of the mixing chamber;generating first sensor data, using a first sensor configured to detect the first component inside the mixing chamber, indicative of a first concentration of the first component in the mixing chamber;controlling, based at least in part on the first sensor data, the first MFC to control the flow of first gas and the first component and thereby causing a first desired concentration of the first component to be in the mixing chamber; andflowing a testing mixture comprising the first gas, the second gas, and the first component from the mixing chamber to a sample chamber through a first outlet flowpath fluidically connecting the mixing chamber and the sample chamber.
18. The method of claim 17, further comprising:flowing gas from the sample chamber to a sensor chamber through a second outlet flowpath, wherein a second sensor is coupled to the sensor chamber and configured to detect aDocket No. BLUCP027WOsecond component in the sensor chamber and generate second sensor data indicative of a second amount of the second component in the sensor chamber; andgenerating the second sensor data, by the second sensor, indicative of the second amount of the second component in the sensor chamber.
19. The method of claim 18, wherein:the first outlet flowpath further comprises a first valve having a first valve inlet, a first valve outlet, and a second valve outlet, wherein a sample chamber inlet is fluidically connected to the first valve outlet,the second outlet flowpath further comprises a second valve having a second valve inlet, a third valve inlet, and a third valve outlet, wherein a sample chamber outlet is fluidically connected by the second outlet flowpath to the third valve inlet of the second valve,a bypass flowpath spans from, and fluidically connects, the second valve outlet of the first valve to the second valve inlet of the second valve, andthe method further comprises:flowing the testing mixture to the sample chamber and the sensor chamber, and not the bypass flowpath, by positioning the first valve in a first configuration and thereby causing the testing mixture to flow through the first valve inlet and flow out the first valve outlet to the sample chamber, and by positioning the second valve in a third configuration and thereby causing the gas flowing from the sample chamber to flow through the third valve inlet to flow out the third valve outlet to the sensor chamber; andflowing the testing mixture to the bypass flowpath and the sensor chamber, and not to the sample chamber, by positioning the first valve in a second configuration and thereby causing the testing mixture to flow through the first valve inlet to flow out the second valve outlet to the bypass flowpath, and by positioning the second valve in a fourth configuration and thereby causing gas flowing in the bypass flowpath to flow through the third valve inlet to flow out the third valve outlet to the sensor chamber.
20. The method of claim 18, further comprising generating, by a third sensor coupled to the sensor chamber and configured to detect the first component in the sensor chamber, third sensor data indicative of the first component in the sensor chamber.Docket No. BLUCP027WO21. The method of claim 17, further comprising:flowing, by a third MFC, a third gas and a third component through a third flowpath to a third inlet of the mixing chamber;generating fifth sensor data, using a fifth sensor configured to detect the third component inside the mixing chamber, indicative of a third concentration of the third component in the mixing chamber;controlling, based at least in part on the fifth sensor data, the third MFC to control the flow of third gas and the third component and thereby causing a third desired concentration of the third component to be in the mixing chamber; andthe flowing the testing mixture further comprises flowing the first gas, the second gas, the first component, the third gas, and the third component from the mixing chamber to the sample chamber through the first outlet flowpath.