Method for producing a product from a liquid mixture by a heating assembly in a processing system - Patent Application 20070122997
The processing system using assist gas flow in a reaction chamber addresses the inefficiencies of conventional lithium-ion battery material production by enabling rapid, energy-efficient, and high-quality production of structured active materials with enhanced electrode density and energy density.
Patent Information
- Application Number
- JP2023217796
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2020-06-28
- Filing Date
- 2023-12-25
- Publication Date
- 2025-12-23
- Estimated Expiration
- 2040-06-29
AI Technical Summary
Conventional processes for producing lithium-ion battery materials, particularly cathode active materials, are costly, time-consuming, and result in inconsistent quality due to high energy consumption, long reaction times, and poor yield, leading to challenges in achieving uniform particle size, morphology, and stoichiometry.
A processing system utilizing an assist gas flow within a reaction chamber to produce particulate materials from a liquid mixture, allowing for continuous production of high-quality, structured active materials by mixing precursor compounds in a liquid form with gases to form a homogenous gas-solid mixture, which is then processed into dry solid particles with desired crystal structure and morphology.
This method significantly reduces production time and energy consumption while achieving high-quality, uniform active battery materials with improved electrode density and energy density compared to conventional methods.
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Abstract
Description
[Technical Field]
[0001] CROSS-REFERENCE TO RELATED APPLICATIONS This application claims the benefit of U.S. Provisional Patent Application Publication No. 62 / 868,843, filed June 28, 2019. All of the above applications are incorporated herein by reference.
[0002] The present invention relates generally to the preparation of materials for use in batteries, and more particularly to processing systems and methods for producing structured cathode or anode active materials for use in secondary batteries. [Background technology]
[0003] Much effort is being expended in developing advanced electrochemical battery cells to meet the growing demands in various consumer electronics, electric vehicles, and grid energy storage applications for high energy density, high power performance, large capacity, long cycle life, low cost, and high safety. In many cases, it is desirable to make batteries small, lightweight, and rechargeable (and thus reusable) to conserve space and material resources.
[0004] In electrochemically active battery cells, the cathode and anode are immersed in an electrolyte and electronically separated by a separator. The separator is typically made of a porous polymer membrane material, so that metal ions released from the electrodes into the electrolyte can diffuse through the separator's pores and migrate between the cathode and anode during battery charging and discharging. Battery cell types are typically named for the metal ions transported between their cathode and anode electrodes. Various rechargeable secondary batteries, such as nickel-cadmium batteries, nickel-metal hydride batteries, lead-acid batteries, lithium-ion batteries, and lithium-ion polymer batteries, have been developed for commercial use over the years. For commercial use, rechargeable secondary batteries are required to have high energy density, high power density, and be safe. However, a trade-off exists between energy density and power density.
[0005] Lithium-ion batteries are secondary batteries developed in the early 1990s. Compared to other secondary batteries, lithium-ion batteries offer high energy density, long cycle life, no memory effect, low self-discharge rate, and environmental benefits. Lithium-ion batteries have rapidly gained acceptance and have come to dominate the secondary battery sales market. However, the cost of producing various lithium battery materials for sale is significantly higher than other types of secondary batteries.
[0006] In lithium-ion batteries, the electrolyte primarily consists of a lithium salt (e.g., LiPF6, LiBF4, or LiClO4) in an organic solvent (e.g., ethylene carbonate, dimethyl carbonate, and diethyl carbonate) that allows lithium ions to move freely through the solvent. Typically, aluminum foil (e.g., 15–20 μm thick) and copper foil (e.g., 8–15 μm thick) are used as the current collectors for the cathode and anode electrodes, respectively. For the anode, micron-sized graphite (with a reversible capacity of approximately 330 mAh / g) is often used as the active material coated on the anode current collector. Graphite materials are often prepared from solid-state processes such as grinding and pyrolysis at extremely high temperatures (e.g., graphitization at approximately 3000 °C) without oxygen. Similar to active cathode materials, various solid-state materials with different crystal structures and capacities have been developed over the years. Examples of good cathode active materials include nanometer or micron sized lithium transition metal oxide materials and lithium ion phosphate.
[0007] The cathode active material is the most expensive component of a lithium-ion battery and determines, to a relatively large extent, the energy density, cycle life, manufacturing cost, and safety of a lithium battery cell. When lithium batteries were first commercialized, lithium cobalt oxide (LiCoO2) material was used as the cathode material, and it still holds a significant market share in the cathode active material market. However, cobalt is toxic and expensive. Other lithium transition metal oxide materials, such as layered LiMeO2 (where the metal Me = Ni, Mn, Co, etc.), have been used, such as LiNiO2, which has a reversible capacity of about 140-150 mAh / g / practical capacity. 0.33 Mn 0.33 Co 0.33 Recently, lithium metal phosphates (e.g., LiFePO4, approximately 140-150 mAh / g) have been developed as active cathode materials. When used as cathode materials, spinel-structured LiMnO4 materials exhibit poor battery cycle life, while olivine-structured LiFePO4 materials suffer from low energy density and poor low-temperature performance. While LiMeO2 materials have good electrochemical performance, previous LiMeO2 manufacturing processes can result in agglomerates, resulting in lower electrode densities compared to LiCoO2. In either case, previous processes for producing materials for use in batteries (especially cathode active materials) are costly due to the lengthy process times and significant energy consumption. Furthermore, previous material quality is inconsistent and manufacturing yields are poor.
[0008] Conventional material manufacturing processes, such as solid-state reactions (e.g., mixing solid precursors followed by calcination) and wet chemical processes (e.g., processing precursors in solution via coprecipitation, sol-gel, or hydrothermal reaction, followed by mixing and calcination), present significant challenges in creating nanostructured and microstructured materials. Consistently producing uniform solid materials (i.e., particles and powders) with desired particle size, morphology, crystalline structure, particle shape, and even desired stoichiometry is difficult. Most conventional solid-state reactions require long calcination times (e.g., 4–20 hours) and additional annealing processes to ensure complete reaction, homogeneity, and grain growth. For example, spinel-structured LiMn2O4 and olivine-structured LiFePO4 materials produced by solid-state reactions require at least several hours of calcination in addition to a separate post-thermal annealing process (e.g., 24 hours), yet still exhibit poor quality consistency. One inherent problem associated with solid-state reactions is the presence of temperature and chemical gradients (such as O2) inside the calciner, which limits the performance, consistency, and overall quality of the final product.
[0009] On the other hand, wet chemical processes, which are performed at low temperatures, typically involve fast chemical reactions but require a separate high-temperature firing process and even an additional annealing process at a later time. Furthermore, the chemical additives, gelling agents, and surfactants required in wet chemical processes add to the cost of material production (in purchasing additional chemicals and adjusting specific process sequences, ratios, pH, and temperatures) and can also affect the final composition of the resulting active material (thus often requiring additional steps to remove unwanted chemicals or filter the product). Furthermore, the primary particle size of the product powder produced by wet chemistry is very small and tends to aggregate into undesirably larger secondary particles, thereby affecting the energy packing density. Furthermore, the morphology of the resulting powder particles often exhibits undesirable amorphous aggregates, porous aggregates, wire-like shapes, rod-like shapes, flakes, etc. Uniform particle size and shape, which allows for high packing density, are desirable.
[0010] The synthesis of lithium cobalt oxide (LiCoO) materials is relatively simple and involves mixing a lithium salt (e.g., lithium hydroxide (LiOH) or lithium carbonate (LiCO)) with cobalt oxide (CoO) of the desired particle size, followed by furnace firing at very high temperatures for extended periods (e.g., 900°C for 20 hours) to ensure that the lithium metal diffuses into the cobalt oxide crystalline structure and forms the appropriate final product of LiCoO powder with a layered crystalline structure. This approach does not work for LiMeO because transition metals such as Ni, Mn, and Co do not diffuse well into each other and do not form a uniformly mixed transition metal layer when their oxides or salts are directly mixed and reacted (solid-state firing). Therefore, conventional LiMeO2 manufacturing processes require purchasing or preparing transition metal hydroxide precursor compounds (e.g., Me(OH)2, Me=Ni, Mn, Co, etc.) from a wet chemical process of co-precipitation before making the final active cathode material (e.g., lithium NiMnCo transition metal oxide (LiMeO2)).
[0011] Because the water solubility of these Ni(OH)2, Co(OH)2, and Mn(OH)2 precursor compounds differs and they typically precipitate at different concentrations, the pH of the mixed solution of these precursor compounds must be adjusted, and ammonia (NH3) or other additives must be added slowly in small aliquots to ensure that nickel (Ni), manganese (Mn), and cobalt (Co) co-precipitate to form micron-sized nickel-manganese-cobalt hydroxide (NMC(OH)2) secondary particles. Such co-precipitated NMC(OH)2 secondary particles are often aggregates of nanometer-sized primary particles. Therefore, the final lithium NMC transition metal oxide (LiMeO2) made from the NMC(OH)2 precursor compound is also an aggregate. These aggregates tend to break up under high pressure during the electrode calendaring step and coating onto current collector foils. Therefore, when these lithium NMC transition metal oxide materials are used as cathode active materials, relatively low pressures must be used in the calendaring step, further limiting the electrode density of the resulting cathode.
[0012] In the conventional manufacturing process for LiMeO2 active cathode material, precursor compounds such as lithium hydroxide (LiOH) and transition metal hydroxide (Me(OH)2) are homogeneously mixed in solid form and stored in a thick Al2O3 crucible. The crucible is then placed in a furnace with a temperature ramp rate of 5–10 °C / min until the temperature reaches 900–950 °C and sintered for 10–20 hours. Because the precursor compounds are heated at high temperatures for long periods, adjacent particles sinter together, and a milling step is often required after sintering. Therefore, particles of undesired sizes must be screened and removed after milling, further reducing the overall yield. High temperatures and long reaction times also result in the evaporation of lithium metal, typically requiring the addition of an additional amount of lithium precursor compound (e.g., 10%) during sintering to ensure the final product has the correct lithium metal / transition metal ratio. Overall, such multi-step batch manufacturing processes are quite labor-intensive and energy-consuming, with process times of up to one week. Batch processes also increase the opportunity for impurities due to poor quality consistency in run-to-run control and low overall yields.
[0013] Therefore, there is a need for improved processes and systems for producing high quality, structured active materials for battery cells. [Prior art documents] [Patent documents]
[0014] [Patent Document 1] U.S. Provisional Patent Application Publication No. 62 / 868843 [Patent Document 2] US Patent Application Publication No. 16 / 457885 [Patent Document 3] US Patent Application Publication No. 16 / 457889 Summary of the Invention [Means for solving the problem]
[0015] The present invention relates generally to a processing system that uses an assist gas flow inside a reaction chamber of the processing system and a method for producing particulate material from a liquid mixture in the processing system. More specifically, the present invention relates to a method and processing system for producing material particles (e.g., active electrode material, etc.) with desired crystal structure, crystal size, and crystal morphology.
[0016] In one embodiment, a processing system for producing a particulate material from a liquid mixture is provided. The processing system includes one or more gas lines, a system inlet connected to the one or more gas lines that deliver one or more gases to the processing system, and one or more power jet modules adapted to eject the liquid mixture into one or more droplet streams and eject the one or more droplet streams into the processing system. The processing system further includes a reaction chamber adapted to process the reaction mixture into a product, and a heating assembly.
[0017] In one aspect, the heating assembly includes a second gas line connected to an opening in a chamber wall of the reaction chamber to deliver one or more second gas streams to the reaction chamber, and a gas delivery element connected to the second gas line and positioned inside the reaction chamber. In another aspect, the reaction mixture includes one or more first gas streams, one or more second gas streams, and one or more droplet streams. In another aspect, the processing system further includes a dispersion chamber connected to the one or more power jet modules and adapted to disperse the one or more droplet streams together with the one or more gas streams.
[0018] In yet another aspect, the treatment system further includes a buffer chamber adapted to deliver one or more gas streams flowing from the system inlet to the dispersion chamber. In another embodiment, the buffer chamber further includes a gas distributor having one or more channels therein for delivering one or more gases to the plurality of gas streams. In another embodiment, the gas distributor is shaped to fit the inner periphery of the chamber wall of the buffer chamber. In yet another aspect, the treatment system further includes one or more gases and one or more droplet streams flowing relative to each other inside the dispersion chamber at an angle between 0 degrees and about 180 degrees. In one embodiment, the gas delivery element of the treatment system is adapted to mix the gas stream with one or more droplet streams generated from the one or more power jet modules, and the gas stream and the one or more droplet streams flow relative to each other inside the dispersion chamber at an angle between 0 degrees and about 180 degrees.
[0019] In another embodiment, a processing system for producing a product is provided, comprising: one or more first gas lines; a system inlet connected to the one or more first gas lines that deliver one or more first gas streams to the processing system; one or more power jet modules adapted to eject a liquid mixture into one or more droplet streams and eject the one or more droplet streams into the processing system; a dispersion chamber connected to the one or more power jet modules and adapted to disperse the one or more droplet streams with the one or more first gas streams into a gas-liquid mixture, wherein the one or more first gas streams and the one or more droplet streams flow relative to one another at a dispersion angle (α) of 0 degrees to about 180 degrees; a reaction chamber adapted to process the reaction mixture into a product; and a heating assembly. In one aspect, one or more second gas streams are delivered by a gas delivery element and intermix with the one or more gas-liquid mixture streams inside the reaction chamber at an angle (β) of 0 degrees to about 180 degrees.
[0020] In another embodiment, a method for producing a product from a liquid mixture is provided. The method includes delivering one or more first gas streams to a buffer chamber of a processing system via a system inlet, delivering one or more second gas streams to a reaction chamber of the processing system via a heating assembly, jetting the liquid mixture into one or more droplet streams with one or more power jet modules of the processing system, causing the one or more droplet streams to flow inside a dispersion chamber of the processing system via the one or more power jet modules, and forming a reaction mixture inside the reaction chamber, the reaction mixture including the one or more first gas streams, the one or more second gas streams, and the one or more droplet streams. The method may also include heating the reaction chamber of the processing system using one or more second gas streams heated to a temperature between 100°C and 1400°C, and processing the reaction mixture into a product inside the reaction chamber.
[0021] So that the above-recited features of the invention can be understood in detail, a more particular description of the invention briefly summarized above can be made by reference to several embodiments, some of which are illustrated in the accompanying drawings. It should be noted, however, that the accompanying drawings illustrate only typical embodiments of the invention and are therefore not to be considered as limiting the scope of the invention, as other embodiments may be recognized that are equally effective for the invention. [Brief explanation of the drawings]
[0022] [Figure 1A] FIG. 1 is a perspective view of an embodiment of an example processing system that uses an assist gas flow inside a reaction chamber. [Figure 1B] 10 is a cross-sectional view of another embodiment of another example processing system using an assist gas flow inside the reaction chamber. [Figure 1C] 1 is a cross-sectional view of an apparatus that can be used in a processing system that uses an assist gas flow inside a reaction chamber. [Figure 2A] 1 is a cross-sectional view of a dispersion chamber of the apparatus that can be used in a processing system that uses an assist gas flow inside the reaction chamber. [Figure 2B]10 illustrates the angle between the gas flow and the droplet flow inside the dispersion chamber according to one embodiment of the present invention. [Figure 3A] 1 is a cross-sectional view of a reaction chamber of an apparatus that can be used in a processing system that uses an assist gas flow inside the reaction chamber. [Figure 3B] 1 illustrates the angle between the gas-liquid mixture and the heated gas flow inside the reaction chamber according to one embodiment of the present invention. [Figure 4] A method for producing a particulate material is presented. [Figure 5] 1 illustrates velocity vectors within a processing system that can be used in the device, according to one embodiment of the present invention. [Figure 6] 1 illustrates velocity streamlines within an apparatus that can be used in a processing system, according to one embodiment of the present invention. [Figure 7] 1 illustrates the temperature distribution of an apparatus that can be used in a processing system that uses an assist gas flow inside a reaction chamber, according to one embodiment of the present invention. [Figure 8] 1 illustrates velocity streamlines within an apparatus that can be used in a processing system, according to one embodiment of the present invention. [Figure 9] 1 illustrates the temperature distribution of an apparatus that can be used in a processing system that uses an assist gas flow inside a reaction chamber, according to one embodiment of the present invention. DETAILED DESCRIPTION OF THE INVENTION
[0023] The present invention generally provides a processing system that uses an assist gas flow inside a reaction chamber of the processing system and a method for producing a particulate material from a liquid mixture in the processing system. The processing system is useful for performing a continuous process to produce the particulate material, saving material production time and energy and solving problems such as high production costs, low yields, poor quality consistency, low electrode density, and low energy density encountered in conventional active material manufacturing processes. The processing system generally includes a system inlet for delivering one or more gases through one or more gas lines, a buffer chamber, a dispersion chamber coupled to one or more power jet modules, a reaction chamber, a heating assembly inside the reaction chamber, and a system outlet for delivering the particulate material out of the processing system.
[0024] In one aspect, precursor compounds, such as metal-containing precursors, are mixed into a liquid mixture, so that the ratio of different metal precursors can be adjusted as desired and a homogeneous mixture of precursors can be obtained. The liquid mixture is then immediately mixed with a gas to form a homogeneously mixed gas-solid mixture, which is continuously processed in the gas phase by a heated gas to react into dry solid particles of particulate material inside a reaction chamber.
[0025] In another embodiment, a homogenous mixture of metal precursor compounds in a desired ratio is mixed into a liquid mixture and injected into a dispersion chamber, which receives one or more gases (e.g., carrier gas, reactant gas, oxidizing gas, oxygen gas, etc.) from a buffer chamber, thereby forming droplets of the gas-liquid mixture within the dispersion chamber before entering the reaction chamber.
[0026] In one embodiment, droplets of the gas-liquid mixture flow into a reaction chamber and are processed to become a gas-solid mixture, and heated air or heated gas actively flows through a heating assembly into the interior chamber space inside the reaction chamber, so that the heated gas can act as both a gas source and / or an energy source for various reactions (drying reactions, oxidation reactions, heating reactions, etc.) inside the reaction chamber.
[0027] The reaction products (e.g., particles, battery oxide materials, particulate materials, etc.) emerging from the reaction chamber are delivered out of the reaction chamber and cooled. After cooling, the reaction products comprise solid material particles or fine powders of the oxide form of the precursor composition (e.g., metal oxide materials, such as fine powders of mixed metal oxide materials) with the desired crystal structure, particle size, and morphology. Thus, high quality and uniform active battery materials can be obtained with significantly less time, labor, and monitoring than materials prepared from conventional manufacturing processes.
[0028] In one embodiment, the heating assembly includes a gas line connected to an opening in the chamber wall of the reaction chamber for delivering one or more heated gases (e.g., gases heated to temperatures between 100°C and 1400°C) to the reaction chamber. The one or more heated gases can serve as an energy source for reactants (e.g., reaction mixtures, gas-liquid mixtures, liquid mixtures, and other mixtures) reacting within the reaction chamber when such gas streams are heated before entering the processing system. The heating assembly further includes a gas delivery element connected to the gas line for delivering the one or more heated gases, positioned inside the reaction chamber, and extending to an inlet region of the reaction chamber, which is connected to the dispersion chamber. The reaction chamber is further connected to a system outlet for delivering particulate material out of the processing system.
[0029] In another embodiment, one or more gas streams (e.g., carrier gas, oxygen gas, inert gas, nitrogen gas, etc., at temperatures between 200°C and 400°C) are delivered to the processing system through a system inlet and serve as a gas source for forming a gas-liquid mixture with the liquid mixture and as a carrier gas for delivering the gas-liquid mixture to the reaction chamber. The gases can also serve as an energy source for the gas-liquid mixture to react in the reaction chamber if such gases are heated to temperatures above 20°C (e.g., between 100°C and 400°C) before entering the processing system.
[0030] In yet another embodiment, a liquid mixture, which may be a metal-containing liquid mixture, is immediately jetted into a droplet stream by one or more power jet modules connected to a dispersion chamber, which is then dispersed in the dispersion chamber of the processing system. The droplet stream is continuously mixed with a gas to form a gas-liquid mixture, which is then flowed and delivered to the reaction chamber.
[0031] In one embodiment, inside the reaction chamber, one or more heated gas streams are actively delivered thereto, and the gas-liquid mixture mixes together inside the interior chamber space of the reaction chamber to form a reaction mixture. In another embodiment, the one or more heated gas streams delivered to the reaction chamber are heated to a desired reaction temperature (such as 100°C to 1400°C, e.g., 300°C to 1000°C, or 400°C to 800°C). In yet another embodiment, the reaction chamber of a processing system can be heated to a reaction temperature by using one or more gases heated to a temperature of 100°C to 1400°C. The reaction mixture inside the reaction chamber is processed into products inside the reaction chamber at the reaction temperature over a reaction period and delivered out of the reaction chamber. By way of example, the reaction mixture can include a mixture of one or more liquids, one or more gases, one or more droplet streams, and a heated gas, and combinations thereof.
[0032] Processing system using assist gas flow inside a reaction chamber of the processing system - Patents.com
[0033] 1A is a perspective view of an exemplary embodiment of a processing system 100 provided in a method for generating a particulate material from a liquid mixture therein. The processing system 100 may generally include a system inlet 102, a system outlet 104, a reaction chamber 110, and a heating assembly 180. The heating assembly 180, which will be described in detail below, is designed to provide an assist gas flow inside the reaction chamber 110 of the processing system 100.
[0034] A system inlet 102 is provided for delivering one or more gases, such as carrier gases and other gases, to the processing system 100 through gas lines 106. A system outlet 104 is connected to a reaction chamber 110 for delivering particulate material out of the processing system 100 after processing reactants, such as a liquid mixture of chemical solutions (e.g., a mixture of liquid battery reactants and chemical solutions), into products (e.g., battery particulate material, battery cathode material, battery anode material, etc.).
[0035] 1A, the processing system 100 may further include at least one buffer chamber 130, which is connected to the system inlet 102 and accommodates channels (e.g., one or more channels) of one or more gas distributors or gas distribution mechanisms therein for redirecting one or more gas streams (e.g., one or more gases F1 shown in FIG. 1B) received from the system inlet 102 into multiple uniform gas streams (e.g., one or more gas streams F2 shown in FIG. 1B) flowing inside the processing system 100. The one or more gases flowing inside the buffer chamber 130 may be selected from gas sources of air, oxygen, carbon dioxide, nitrogen gas, hydrogen gas, inert gases, noble gases, and combinations thereof, among others.
[0036] Additionally, the processing system 100 may also include a dispersion chamber 120 coupled to one or more power jet modules (e.g., power jet modules 140A, 140B, 140C, etc.) provided for receiving one or more chemical reactants, mixing the chemical reactants into one or more liquid mixtures, and ejecting the one or more liquid mixtures into the dispersion chamber 120, thereby delivering the one or more liquid mixtures to the dispersion chamber 120 of the processing system 100.
[0037] The power jet modules 140A, 140B, 140C, etc., are attached to a portion of the dispersion chamber and can use air pressure to eject the liquid mixture and convert it directly into a vapor containing small droplets inside the dispersion chamber. Alternatively, the vapor can be generated outside the dispersion chamber 120 and delivered to the dispersion chamber 120. Depending on the selection of the power jet module used, the liquid mixture compound, the temperature of the dispersion chamber 120, the gas flow rate, and the residence time inside the dispersion chamber, the appropriate droplet size can be adjusted. By way of example, vapor with liquid droplet sizes between 0.1 microns and 1 millimeter can be generated inside the dispersion chamber.
[0038] The number of power jet modules that can be coupled to the dispersion chamber 120 is not limited and can be one, two, three, or any number of power jet modules coupled to the dispersion chamber 120 according to custom design or as needed. In one embodiment, two or more power jet modules are positioned around the periphery of the dispersion chamber 120. Each power jet module is adapted to eject a liquid mixture into one or more droplet streams into the dispersion chamber 120, whereby the one or more droplet streams are mixed with one or more gases passing through one or more channels of the gas distribution mechanism of the buffer chamber 130, thereby forming one or more gas-liquid mixtures inside the dispersion chamber 120 and delivered to the reaction chamber 110.
[0039] In one embodiment, the power jet module 140A is coupled to a portion of the dispersion chamber 120 and generates a vapor of the liquid mixture (e.g., a large volume of small droplets) directly within the dispersion chamber. Generally, the power jet module 140A is capable of generating a vapor of uniform droplets. In another embodiment, the dispersion chamber 120 is connected to one or more power jet modules 140A, 140B, and 140C for receiving the multiple uniform gas streams from the buffer chamber 130 and dispersing the multiple uniform gas streams with one or more droplet streams jetted from an arrangement of one or more power jet modules 140A, 140B, and 140C.
[0040] Furthermore, in one embodiment, a liquid mixture is prepared from two or more precursor compounds and then converted into droplets, each droplet having two or more precursors uniformly distributed together. The water content of the liquid mixture is then removed by passing the droplets through a dispersion chamber, and a gas flow is used to transport the vapor into the dispersion chamber for a suitable residence time. It is further contemplated that the concentration of the precursor compounds in the liquid mixture and the droplet size of the vapor from the liquid mixture can be adjusted to control the chemical composition, particle size, and particle size distribution of the final product particles of the battery material.
[0041] In one embodiment, the reaction chamber 110 of the processing system 100 is provided to receive one or more droplet streams of gas-liquid mixtures and process one or more gas-liquid mixtures delivered from the dispersion chamber 120 by reacting the gas-liquid mixtures with one or more heated gases to oxidize and heat the gas-liquid mixtures into a final reaction product (e.g., battery particle material, oxidized metal oxide material, etc.).
[0042] In another embodiment, the reaction chamber 110 is connected to a heating assembly 180 that uses an assist gas flow therein to deliver heated gas from a gas line 186 connected to the heating assembly 180, with a portion of the heating assembly 180 positioned within the interior chamber space of the reaction chamber 110. The heating assembly 180 is connected to the reaction chamber 110 through an opening 119 located in a chamber wall 118 of the reaction chamber 110.
[0043] The heating assembly 180 includes a gas delivery element 184 within the interior chamber space of the reaction chamber 110. In one embodiment, the gas delivery element 184 is designed to provide a source of dry heat and / or gas to the reactants inside the reaction chamber 110. It is contemplated that an opening in the gas delivery element 184 may be positioned near the connection between the dispersion chamber 120 and the reaction chamber 110 to process the gas-liquid mixture received from the dispersion chamber 120 inside the reaction chamber 110.
[0044] Walls 188 of gas delivery element 184 of heating assembly 180 are provided to channel a gas flow of heated gas received from gas line 186, the gas flow flowing through gas delivery element 184 extending to an inlet region between reaction chamber 110 and dispersion chamber 120. This then causes the heated gas delivered from gas delivery element 184 of heating assembly 180 to flow out of gas delivery element 184 of heating assembly 180 and fill the interior chamber space within chamber wall 118 of reaction chamber 110.
[0045] In one embodiment, gas delivery element 184 is preferably positioned facing upward inside reaction chamber 110. In another embodiment, gas delivery element 184 can be positioned at any angle relative to the ground ranging from 0 degrees to 90 degrees. In one aspect, gas delivery element 184 is perpendicular to the ground. In another aspect, gas delivery element 184 can be at any angle relative to the ground ranging from 0 degrees to 90 degrees.
[0046] 1B is a cross-sectional view of an exemplary processing system 200 that can be used to implement a fast, simple, continuous, and low-cost manufacturing process to produce battery particle material. Processing system 200 includes a system inlet 202 for delivering one or more gases to processing system 200, a buffer chamber 230 connected to system inlet 202, a dispersion chamber 220 connected to buffer chamber 230, a heating assembly 280, a reaction chamber 210 connected to dispersion chamber 220, and a system outlet 204 connected to reaction chamber 210 for delivering the resulting particle material out of processing system 200.
[0047] The system inlet 202 is provided for delivering one or more gases F1 to the buffer chamber 230. The one or more gases F1 are pressurized downward and flow at a constant gas velocity through the gas distributor 232 of the buffer chamber 230, thereby directing and distributing the one or more gases F1 into multiple uniform gas flows F2 out of the buffer chamber 230 and into the dispersion chamber 220. The gas distributor 232 may have one or more channels 234 arranged in a circular phase to direct the gas flows. For example, the channels 234 of the gas distributor 232 may be arranged like a showerhead so that the gas flow F1 can be distributed into multiple uniform gas flows F2. In one embodiment, the one or more gases F1 may be pumped through an air filter to remove any particles, droplets, or contaminants, and the flow rate of the gas F1 may be adjusted by a valve or other means. In one embodiment, the flow rate of the multiple uniform gas flows F2 emerging from the channel 234 is greater than the flow rate of the one or more gases F1. Furthermore, the gas gathers and concentrates in the direction of the multiple uniform gas flows F2.
[0048] 1C is an example cross-sectional view (cross-section taken along dashed line B-B' in FIG. 1B) of buffer chamber 230, according to one embodiment of the present invention. Gas distributor 232 of buffer chamber 230 is located at the bottom of buffer chamber 230 and includes multiple channels 234 within the interior of chamber wall 238 of buffer chamber 230, provided to direct gas F1 received from system inlet 202 into multiple integrated gas flows F2. Channels 234 of gas distributor 232 allow one or more gases to pass in a unified direction and at a desired uniform flow rate.
[0049] The one or more gases F1 can be one or more carrier gases, such as air, oxygen, carbon dioxide, nitrogen gas, hydrogen gas, an inert gas, a noble gas, and combinations thereof, among others. The one or more gases selected can be one or more gases that do not react with the droplet stream but that sufficiently mix with the droplet stream of battery metal precursors. In some cases, the chemicals of the droplet stream may react with gas F1 and / or gas F2 to some extent during mixing and / or other reactions inside the dispersion chamber, depending on the temperature of gas F1 and / or gas F2 and the chemical composition of the droplet stream. Furthermore, the residence time of the gas-liquid mixture of the thoroughly mixed droplet stream compounds inside the dispersion chamber 220 can be adjusted and can range from 1 second to 1 hour, for example, depending on the flow rates of the one or more gases F1 and F2 and the path length the droplet stream must travel through the dispersion chamber 220.
[0050] In one embodiment, the dispersion chamber 220 of the processing system 200 is connected to one or more power jet modules (e.g., power jet modules 240A, 240B, etc.) attached to the periphery of the chamber wall 228 of the dispersion chamber 220. FIG. 2A is a cross-sectional view (taken along dashed line A-A' in FIG. 1B) of the dispersion chamber 220 configured in the processing system 200, according to one embodiment of the present invention. In one embodiment, an array of one or more power jet modules (e.g., four power jet modules 240A, 240B, 240C, and 240D shown in FIG. 2A, or five or more power jet modules (not shown)) can be attached to the chamber wall 228 of the dispersion chamber 220 symmetrically (also shown in FIG. 2A) or in other ways (e.g., the power jet modules can be stacked, interleaved, etc., or arranged in other ways).
[0051] 2A, one or more openings 222A, 222B, 222C, and 222D in chamber wall 228 of dispersion chamber 220 are connected to power jet modules 240A, 240B, 240C, and 240D, respectively. In one example, power jet modules 240A, 240B, 240C, and 240D can be attached to chamber wall 228 of dispersion chamber 220 in one arrangement shown in FIG. 2A. In that arrangement, each of the four power jets can be configured on chamber wall 228 adjacent to and evenly spaced from one another on the same horizontal line of chamber wall 228.
[0052] Each of the power jet modules 240A, 240B, 240C, and 240D includes a power jet 242A, 242B, 242C, and 242D, respectively, for ejecting the liquid mixture supplied to the power jet module 240A into one or more droplet streams. Each of the power jet modules 240A, 240B, 240C, and 240D may further include a support frame for supporting the power jet module 240A, 240B, 240C, and 240D, respectively, a module actuator 246A, 246B, 246C, and 246D, and a connector 245A, 245B, 245C, and 245D. Each of the module actuators 246A, 246B, 246C, and 246D, respectively, controls the one or more droplet streams F ejected from each of the power jets 242A, 242B, 242C, and 242D. A , F B , F C , F D and is mounted inside its own support frame for moving and pushing into dispersion chamber 220. Connectors 245A, 245B, 245C, 245D are each provided for connecting a module actuator 246A, 246B, 246C, 246D and a power jet 242A, 242B, 242C, 242D, respectively.
[0053] In one example, power jets 242A, 242B, 242C, 242D are positioned near the sides of dispersion chamber 220 and direct droplet stream F, as shown in FIG. A ~F Dis injected horizontally into the dispersion chamber 220 and passes through the dispersion chamber horizontally and laterally. For example, when the dispersion chamber 220 (e.g., a tubular dispersion chamber, etc.) is positioned horizontally and the power jets 242A, 242B, 242C, 242D are positioned near one end of the dispersion chamber 220, the vapor flow delivered from one end of the dispersion chamber 220 through the other end can pass through a path inside the dispersion chamber 220 for the length of its residence time.
[0054] In another example, the power jets 242A, 242B, 242C, 242D are positioned near the top of the dispersion chamber 220 (e.g., a dome-shaped dispersion chamber, etc.) to direct the droplet stream F A , F B , F C , F D is injected vertically into the dispersion chamber 220 and passes vertically downward through the dispersion chamber. Alternatively, the power jets 242A, 242B, 242C, 242D can be positioned near the bottom of the dispersion chamber 220 to inject the droplet stream vertically upward into the dispersion chamber (as shown in FIG. 2B), increasing the residence time of the resulting stream within the dispersion chamber.
[0055] 1B, in addition to the liquid mixture flow, the dispersion chamber 220 is also filled with a gas flow received from the buffer chamber 230. The gas distributor 232 is coupled to an end of the buffer chamber 230 and adapted to flow a plurality of uniform gases F2 into the dispersion chamber 220. Simultaneously with the formation of the droplet flow inside the dispersion chamber 220 as the droplet flow is transported through the dispersion chamber 220, the plurality of uniform gas flows F2 that can be delivered to the dispersion chamber 220 may or may not remove moisture from the vapor, forming one or more gas-liquid mixture flows containing the liquid mixture in the direction of F3. Also, the plurality of uniform gas flows F2 are delivered to the dispersion chamber 220 before the vapor is formed, filling the internal volume of the dispersion chamber 220 and maintaining the temperature T before the droplet flow is generated inside the dispersion chamber 220. D It can be preheated to.
[0056] In one example, the gas distributor 232 is connected to an end of the buffer chamber 230, which is connected to the top of the dispersion chamber 220. The gas distributor 232 delivers multiple uniform gases F2 to the dispersion chamber 220, where the gases F2 mix with the droplet streams generated by the power jet modules 240A, 240B, 240C, and 240D attached to the chamber wall 228 of the dispersion chamber 220. In one embodiment, the multiple uniform gas streams F2 are preheated to a temperature between 20°C and 400°C and mixed with the droplet streams to remove moisture from the droplet streams. In another embodiment, the multiple uniform gas streams F2 are used without preheating, ensuring that the gas-liquid mixture formed inside the dispersion chamber 220 is uniformly mixed with the gas.
[0057] In other embodiments, each of the power jets 242A, 242B, 242C, and 242D may be shaped in various configurations, such as a rectangular parallelepiped configuration with six rectangular faces at right angles to one another, a cylindrical configuration with horizontal parallelepiped faces and a circular or elliptical cross section, and / or combinations thereof. Additionally, each of the power jets 242A, 242B, 242C, and 242D may have a nozzle array on one side of the power jet. In one embodiment, the nozzle array is located on a side of the power jet whose base width is greater than its side length and is comprised of evenly spaced orifices, forming a rectangular shape. In other embodiments, the nozzle array may be comprised of other orifice patterns. Other examples of power jet modules are described in U.S. Patent Application Publication No. 16 / 457,885, filed June 28, 2019, entitled "Processing System and Method for Producing a Particulate Material," and U.S. Patent Application Publication No. 16 / 457,889, filed June 28, 2019, entitled "System with Power Jet Modules and Method thereof," the disclosures of each of which are hereby incorporated by reference in their entirety.
[0058] FIG. 2B shows a fluid flow F of droplets inside dispersion chamber 220. Aand the dispersion angle (α A ) is a three-dimensional perspective view of an example of the dispersion angle α of the droplets. A , F B , F C , F D The flow is measured according to the angle between the direction of the droplet flow F2 and the direction of the gas flow F2. A , F B , F C , F D (For example, droplet flow F A ) and gas flows (e.g., multiple uniform gas flows F2) may collide with each other inside the dispersion chamber 220 at angles between 0 and 180 degrees. A and the air flow of gas flow F2 may flow in a straight line, a spiral, a tangled manner, and / or in other ways.
[0059] In one embodiment, the fluid flow F of droplets A and the gas flow F2 is at an angle α A (0≦α A ≦180°), which may merge (e.g., become parallel) inside the dispersion chamber 220 into one or more mixed flows (e.g., gas-liquid mixture flow F3). A and gas flow F2 may flow at various angles toward each other and / or toward the outer periphery of the chamber body, promoting the formation of spiral, intertwining, and / or other air flows inside the dispersion chamber 220.
[0060] For example, the gas flow and the liquid flow of the droplet stream flowing inside the dispersion chamber 220 can be configured to flow in a co-current manner. The advantages of a co-current flow include, among other things, a shorter residence time, a lower particle drying temperature, and a higher particle separation efficiency. As another example, the liquid flow F of the droplet stream can be configured to flow in a co-current manner. A The gas flow F2 can be configured at an angle α of 180 degrees and flow in a convective manner. The advantages of convection include, among other things, a longer residence time and a higher particle drying temperature. In an alternative embodiment, the dispersion chamber 220 can be positioned horizontally.
[0061] In one example, the droplet stream F A , F B , FC , F D The gas streams are configured at an angle α of less than 90 degrees and may meet inside the dispersion chamber to form a mixed flow of gas-liquid mixture F3. A and gas streams F2 are configured at a 90 degree angle α and may merge inside dispersion chamber 220 into one or more mixed streams (e.g., gas-liquid mixture stream F3). A and gas flow F2 may flow at various angles toward each other and / or toward the outer periphery of the chamber body, promoting the formation of spiral, intertwining, and / or other air flows inside the dispersion chamber 220.
[0062] Referring again to FIG. 1B, once the droplet stream F of the liquid mixture is formed, A , F B , F C , F D When one or more gas-liquid mixtures F3 mix with gas flow F2 to form a gas-liquid mixture, the gas-liquid mixture is delivered to the reaction chamber 210 through the dispersion chamber 220. The reaction chamber 210 of the processing system 200 is connected to the dispersion chamber 220 to receive one or more gas-liquid mixture flows F3 delivered from the dispersion chamber 220. Additionally, the reaction chamber 210 is connected to the heating assembly 280 through an opening 219 in the chamber wall 218 of the reaction chamber 210 to deliver one or more heated gases F6 to the interior chamber space within the reaction chamber 210.
[0063] The heating assembly 280 includes a gas delivery element 284 surrounded by a wall 288 for channeling one or more heated gas streams F6 delivered from a gas line 286. The gas delivery element 284 extends into the interior chamber space of the reaction chamber 210 and is connected at one end to the gas line 286 to deliver the one or more heated gases F6, and extends to an inlet region 212 of the reaction chamber 210, which is adjacent to the dispersion chamber 220. Furthermore, processed products, such as oxide particles, particulate material, etc., are formed near the outlet region 214 and are delivered out of the processing system 200 through a system outlet 204 located near the end of the reaction chamber 210.
[0064] In one embodiment, one or more heated gas streams F6 are delivered through gas delivery element 284 of heating assembly 280 and mixed with one or more gas-liquid mixture streams F3 delivered from distribution chamber 220 at an angle to each other inside reaction chamber 210. The angle between one or more heated gas streams F6 and one or more gas-liquid mixture streams F3 can be between 0 degrees and 180 degrees.
[0065] In one embodiment, one or more gases F6 can be heated before being delivered to the reaction chamber through openings 219 in the chamber wall 218 of the reaction chamber 210. The one or more heated gas streams F6 can be heated by passing through a suitable heating mechanism, such as an electric heater, a fuel-fired heater, or a burner, among other heaters. Furthermore, the one or more heated gas streams F6 can be heated to a temperature between 100°C and 1400°C, e.g., between 300°C and 1000°C, or between 400°C and 800°C, and thus provide sufficient energy as a heat source for the desired reaction within the reaction chamber. The wall 288 of the heating assembly 280 is made of a thermal insulating material (e.g., stainless steel) and can sustain high temperatures in the space enclosed by the wall 288, which can be greater than 100°C, e.g., greater than 300°C, greater than 500°C, or greater than 1000°C, e.g., between 400°C and 800°C.
[0066] In another embodiment, the gas-liquid mixture F3 and the heating gas F6 may impinge on one another near the inlet region 212 inside the reaction chamber 210 and adjacent the dispersion chamber 220. In one example, the gas delivery element 284 of the heating assembly 280 can extend to a location inside the reaction chamber such that the one or more gas-liquid mixture streams F3 impinge on the one or more heating gas streams F6 sufficiently to form a reaction mixture F7 so as to provide sufficient thermal energy for the one or more gas-liquid mixture streams F3 to continuously initiate the desired reaction within the reaction chamber 210 quickly and for a sufficient time and manner. For example, the gas delivery element 284 is preferably positioned close to the inlet region 212 inside the reaction chamber 210, which is adjacent the dispersion chamber 220.
[0067] In one embodiment, gas delivery element 284 is preferably positioned facing upward inside reaction chamber 210 to deliver one or more heated gases F6 to inlet region 212. In another embodiment, gas delivery element 284 can be positioned at any angle relative to the chamber body of reaction chamber 210 ranging from 0 degrees to 90 degrees. In one example, the chamber body of gas delivery element 210 is perpendicular to the ground. In another example, the chamber body of gas delivery element 210 can be positioned at any angle relative to the ground ranging from 0 degrees to 90 degrees.
[0068] 3A is a cross-sectional view (the cross-section indicated by dashed line C-C' in FIG. 1B) of a reaction chamber 210 having a heating assembly 280 for assisting and delivering a heated gas flow therein. The shape of the channel surrounded by the wall 288 of the gas delivery element 284 of the heating assembly 280 can be circular (as shown in FIG. 1B) or other shapes (e.g., oval, rectangular, square, etc.). The diameter of the gas delivery element 284 of the heating assembly 280 can vary such that the ratio of the diameter of the wall 288 of the gas delivery element 284 to the diameter of the chamber body (surrounded by the chamber wall 218) of the reaction chamber 210 is between 1:10 and about 1:1.
[0069] 3B shows a three-dimensional perspective view of the divergence angle of the gas-liquid mixture stream F3 and one or more heated gas streams F6 inside the reaction chamber 210. Inside the reaction chamber 210, the one or more heated gas streams F6 are delivered through the gas delivery element 284 and diverge at an angle β (e.g., β A ) and gas-liquid mixture stream F3. The angle β is measured according to the angle formed by the direction of the heating gas stream F6 and the direction of the gas-liquid mixture stream F3. The gas-liquid mixture stream F3 and one or more gas mixture streams (e.g., one or more heating gas streams F6) may collide with each other inside the reaction chamber 210 at an angle between 0 degrees and 180 degrees. Furthermore, the gas-liquid mixture stream F3 and one or more heating gas streams F6 may flow in a straight line, a spiral, an intertwined manner, and / or other manners.
[0070] In one embodiment, the one or more heated gas streams F6 and the gas-liquid mixture stream F3 are arranged at an angle β A (0≦β A≦180°) and may converge inside the reaction chamber to become reaction mixture F7 (e.g., co-flow) over the reaction period. Additionally, one or more heated gas streams F6 and gas-liquid mixture stream F3 may flow at various angles toward each other and / or toward the periphery of the chamber body to facilitate the formation of spiral, intertwining, and / or other air flows inside the reaction chamber 210. In one embodiment, one or more heated gas streams F6 and gas-liquid mixture stream F3 may flow at angles β A (less than 90 degrees) and meet to form a mixed flow inside the reaction chamber. In another embodiment, one or more heated gas streams F6 and gas-liquid mixture stream F3 may be configured at an angle β (90 degrees) and meet to form a mixed flow inside the reaction chamber. Additionally, one or more heated gas streams F6 and gas-liquid mixture stream F3 may flow at various angles toward each other and / or toward the periphery of the chamber body to facilitate the formation of spiral, intertwining, and / or other air flows inside the reaction chamber 210.
[0071] For example, gas stream F6 and gas-liquid mixture stream F3 inside reaction chamber 210 may flow co-currently and combine into one or more reaction mixture streams F7. In another example, one or more heated gas streams F6 and gas-liquid mixture streams F3 flowing inside reaction chamber 210 may be configured to flow convectionally (e.g., at a 180 degree angle β) and combine into one or more reaction mixture streams F7. In alternative embodiments, dispersion chamber 210 may be positioned horizontally, vertically, or at an angle.
[0072] 1B , the processing system 200 is connected to an electronic control unit 300 with a CPU 340 for automated control of the processing system 200. Each of the power jet modules 240A, 240B, 240C, and 240D is connected to a liquid source 310 that stores a desired amount of the liquid mixture compound, and to the electronic control unit 300 for directing and controlling the delivery of the liquid mixture compound from the liquid source 310 to each of the power jets 242A, 242B, 242C, and 242D. In one configuration, the liquid mixture within the liquid source 310 can be pumped from the liquid source 310 to each of the power jets 242A, 242B, 242C, and 242D. The pumping of the liquid mixture can be configured to achieve good process throughput of the processing system 200, for example, continuously and at a desired delivery rate (e.g., regulated by a throttle valve or other means).
[0073] In one embodiment, the droplet stream (e.g., F A , F B ) and the plurality of uniform gas flows F2 are arranged at a divergence angle α (e.g., α A , α B The gas stream F2 acts as a carrier gas containing one or more gases (e.g., air, oxygen gas, nitrogen gas, inert gas, etc.) to form one or more gas-liquid mixture streams F3. A and F B into the dispersion chamber 220, where a plurality of uniform gas flows F2 and droplet flows F A and finally conveying it to the reaction chamber 210 by forming one or more gas-liquid mixture streams F3 containing
[0074] In one embodiment, the gas streams F1 and F2 can be maintained at a temperature between 20°C and 400°C. In one aspect, the temperature of F2 is maintained between 20°C and 100°C. In another aspect, the temperature of F2 is maintained between 20°C and 200°C. In yet another aspect, the temperature of F2 is maintained between 25°C and 400°C. Furthermore, the dispersion chamber 220 can be maintained at a temperature T D can be maintained.
[0075] The gas-liquid mixture stream F3 and the one or more heated gas streams F6 are mixed together to form a reaction mixture F7 over a reaction period inside the reaction chamber 210. The reaction mixture F7 is a mixture of the gas-liquid mixture F3 (gas streams F1, F2) and the droplet stream (F A , F B , F C , F D The reaction chamber 210 of the processing system 200 can be heated to a reaction temperature T of 100° C. to 1400° C. by using one or more heated gases F6 having a temperature of 100° C. to 1400° C. R In one embodiment, the temperature T R is the temperature T D Higher than.
[0076] In another embodiment, gas stream F6 is heated to a drying or oxidizing temperature and mixed with gas-liquid mixture F3 to remove moisture from gas-liquid mixture F3. It is designed to obtain spherical solid particles from a thoroughly mixed liquid mixture F3 of two or more liquid mixtures. In contrast, conventional solid manufacturing processes involve mixing or grinding a solid mixture of two or more compounds, resulting in a heterogeneous mixture of the two or more mixtures.
[0077] The reaction mixture F7 inside the reaction chamber 210 is processed into products (e.g., a gas-solid mixture of the oxidation reaction mixture mixed with one or more heated gas streams and / or gas-phase by-products, or waste products, etc.), which accumulate near the outlet region 214 and, after a reaction period inside the reaction chamber 210, are delivered out of the processing system 200 via the system outlet 204. The reaction products delivered out of the reaction chamber 210 include solid material particles or fine powders of the oxidized form of the liquid mixture composition (e.g., metal oxide materials, such as fine powders of mixed metal oxide materials) with a desired crystal structure, particle size, and morphology.
[0078] Optionally, in one embodiment, the treatment system 200 further includes a separator connected to the system outlet 204 at the end of the reaction chamber 210 and adapted to collect the treated product stream and separate the treated product into solid particles and waste. Examples of suitable separators include cyclones, electrostatic separators, electrostatic precipitators, gravity separators, inertial separators, membrane separators, fluidized beds, classifiers, electric sieves, impactors, particle collectors, leaching separators, elutriators, air classifiers, leaching classifiers, and combinations thereof, among others.
[0079] The product can be cooled to obtain final solid particles of the desired size, morphology, and crystalline structure, and can be immediately used for further analysis of their properties (e.g., specific capacity, power performance, charging cycling performance of the particulates, etc.), particle size, morphology, crystalline structure, etc., for use in batteries. For example, the product can be cooled slowly to room temperature to avoid interrupting or failing the process of forming its stable energy state with a uniform morphology and desired crystalline structure. Thus, high-quality and uniform active particle material can be obtained with significantly less time, work, and monitoring than materials prepared from conventional manufacturing processes.
[0080] Method for producing particulate material from a liquid mixture in a processing system using an assist gas flow inside a reaction chamber of the processing system - Patents.com
[0081] 4 shows a method 400 for producing a product from a liquid mixture. In step 410, a temperature T ROne or more heated gases having a specific orientation (e.g., .gtoreq.100) flow into a reaction chamber of a processing system through a heating assembly. A heating assembly 280 is provided for connecting a gas line 286 to an opening 219 in a chamber wall 218 of the reaction chamber 210 to deliver the one or more heated gases to the reaction chamber 210. The heated gas from the gas line 206 flows in a channel through the wall 288 into a gas delivery element 284 of the heating assembly 280. In one example, the gas delivery element 284 is preferably positioned to extend to the inlet region 212 of the reaction chamber 210 adjacent to the dispersion chamber. In one embodiment, the gas delivery element 284 is preferably positioned facing upward inside the reaction chamber 210. In another embodiment, the gas delivery element 284 can be positioned at any angle relative to the ground ranging from 0 degrees to 90 degrees.
[0082] One or more heated gas streams are heated to a desired reaction temperature (e.g., 100°C to 1400°C) and flow into the reaction chamber, where they serve as an energy source for drying and / or reacting the gas-liquid mixture into a reaction mixture over a residence time. The advantages of flowing preheated air or gas include, among other things, fast heat transfer, uniform temperature distribution (especially in the high temperature zones), and easy performance enhancement. The residence time can be any residence time required to effect complete reaction of one or more gas-liquid mixture streams, such as, for example, from 1 second to 10 hours, or even longer than 10 hours.
[0083] Exemplary gas streams of one or more heating gases include, but are not limited to, air, oxygen, carbon dioxide, oxidizing gases, nitrogen gas, inert gases, noble gases, and combinations thereof. For oxidation reactions inside the reaction chamber 210, such as forming oxide materials from one or more liquid mixtures, an oxidizing gas can be used as the gas stream. For reduction reactions inside the reaction chamber, a reducing gas can be used as the heating gas. Additionally, the heating gas can be used as a gas source to form a gas-liquid mixture.
[0084] Optionally, one or more gases are delivered to the buffer chamber of the processing system via a system inlet in step 420. The one or more gases may be, for example, air, oxygen, carbon dioxide, nitrogen gas, hydrogen gas, an inert gas, a noble gas, and combinations thereof, among others.
[0085] Step 430 involves jetting the liquid mixture into one or more droplet streams using one or more power jet modules of the processing system. Forming a liquid mixture from two or more precursors. Generally, liquid precursor compounds can be directly prepared to form a liquid mixture at a desired concentration. Solid precursor compounds can be dissolved or dispersed in an appropriate solvent (e.g., water, alcohol, isopropanol, or any other organic or inorganic solvent, and combinations thereof) to form an aqueous solution, slurry, gel, aerosol, or any other suitable liquid mixture. For example, a desired molar ratio of two or more solid precursors can be prepared to form a liquid mixture by, for example, measuring appropriate amounts of two or more solid precursors into a container with an appropriate amount of solvent. Depending on the solubility of the precursors in the solvent, pH, temperature, and mechanical agitation and mixing can be adjusted to obtain a liquid mixture and sufficiently dissolve and / or evenly distribute the precursor compounds.
[0086] In one example, two or more metal-containing precursors are mixed into a liquid mixture to obtain a final reaction product of a mixed metal oxide material. Examples of metal-containing precursors include, but are not limited to, metal salts, lithium-containing compounds, cobalt-containing compounds, manganese-containing compounds, nickel-containing compounds, lithium sulfate (Li2SO4), lithium nitrate (LiNO3), lithium carbonate (Li2CO3), lithium acetate (LiCH2COO), lithium hydroxide (LiOH), lithium formate (LiCHO2), lithium chloride (LiCl), cobalt sulfate (CoSO4), cobalt nitrate (Co(NO3)2), cobalt carbonate (CoCO3), cobalt acetate (Co(CH2COO)2), cobalt hydroxide (Co(OH)2), cobalt formate (Co(CHO2)2), cobalt chloride (CoCl2), manganese sulfate (MnSO4), manganese nitrate (Mn(NO3)2), manganese carbonate (MnCO3), manganese acetate (Mn( Nickel hydroxide (Mn(OH)), manganese formate (Mn(CHO)), manganese chloride (MnCl), nickel sulfate (NiSO), nickel nitrate (Ni(NO), nickel carbonate (NiCO), nickel acetate (Ni(CHCOO)), nickel hydroxide (Ni(OH)), nickel formate (Ni(CHO)), nickel chloride (NiCl), aluminum (Al)-containing compounds, titanium (Ti)-containing compounds, sodium (Na)-containing compounds, potassium (K)-containing compounds, rubidium (Rb)-containing compounds, vanadium (V)-containing compounds, cesium (Cs)-containing compounds, chromium (Cr)-containing compounds, copper (Cu)-containing compounds, magnesium (Mg)-containing compounds, iron (Fe)-containing compounds, and combinations thereof.
[0087] Without wishing to be bound by theory, it is contemplated that to prepare an oxide material containing two or more different metals, two or more metal-containing precursor compounds may be used as the source of each metal element, and all of the required metal elements may first be mixed into a liquid mixture (e.g., a solution, a slurry, or a gel mixture) so that the two or more different metals can be uniformly mixed in the desired ratio. For example, one or more metal salts with high water solubility may be used to prepare the aqueous solution, slurry, or gel liquid mixture. For example, metal nitrates, metal sulfates, metal chlorides, metal acetates, and metal formates may be used. Organic solvents (e.g., alcohol, isopropanol, etc.) may be used to dissolve or disperse metal-containing precursors with low water solubility. In some cases, the pH value of the liquid mixture may be adjusted to increase the solubility of one or more precursor compounds. Optionally, chemical additives, gelling agents, and surfactants (e.g., ammonia, EDTA, etc.) may be added to the liquid mixture to facilitate dissolving or dispersing the precursor compounds in the selected solvent.
[0088] By adjusting the size of the liquid delivery / injection channels in the power jet module, the desired diameter of one or more droplet streams can be adjusted. Diameters of one or more droplet streams ranging from a few nanometers to hundreds of micrometers can be generated. Depending on the selection of the vapor generator used, the liquid mixture compound, the temperature of the dispersion chamber, the gas flow rate, and the residence time inside the dispersion chamber, the appropriate droplet diameter can be adjusted. As an example, vapor with liquid droplet diameters of 0.1 microns to 1 millimeter can be generated inside the dispersion chamber.
[0089] In step 440, one or more droplet streams are ejected by one or more power jet modules into the interior of a dispersion chamber of the processing system, causing the droplet streams to flow. In one configuration, the one or more power jet modules are connected to a liquid source storing a desired amount of the liquid mixed compound and an electronic control unit for directing and controlling the delivery of the liquid mixed compound from the liquid source to the power jets.
[0090] In another configuration, the liquid mixture in the liquid source can be pumped from the liquid source to the power jet. The pump can be configured to deliver the liquid mixture continuously and at a desired rate (e.g., regulated by a throttle valve or other means) to achieve good process throughput for the processing system. In another configuration, the power jet is positioned outside the dispersion chamber, and the liquid flow generated by the power jet is delivered to the dispersion chamber through a chamber inlet.
[0091] In one embodiment, the one or more power jet modules are adapted to eject the liquid mixture into one or more droplet streams and eject the one or more droplet streams into a processing system. In another embodiment, the droplet streams and the one or more gas streams ejected into the dispersion chamber are dispersed at a dispersion angle (α) relative to one another to form one or more gas-liquid mixture streams including gas streams and droplet streams of one or more gases. The one or more gases and the one or more droplet streams flow relative to one another at a dispersion angle (α) between 0 degrees and about 180 degrees.
[0092] In step 450, a temperature T D In one embodiment, the method comprises dispersing one or more gases together with one or more streams of droplets to form a gas-liquid mixture at a temperature T D is maintained at 20°C to 400°C. One or more droplet streams are mixed in the dispersion chamber by flowing one or more gases continuously and / or at adjustably variable flow rates. Simultaneously, droplet streams ejected from the liquid mixture are carried by the gas through a passage in the dispersion chamber as a thoroughly mixed gas-liquid mixture, and as the gas flows more, the gas-liquid mixture is delivered out of the dispersion chamber and continuously delivered to a reaction chamber connected to the dispersion chamber.
[0093] In step 460, a reaction mixture is formed inside the reaction chamber from one or more heated gases provided by the heating assembly and a gas-liquid mixture of gas and droplet streams provided from the dispersion chamber, thereby processing the reaction mixture into products at a reaction temperature inside the reaction chamber.
[0094] In one embodiment, various gases flowing inside the processing system 100, 200 are heated, and the thermal energy of the heated gases can serve as an energy source for carrying out drying, reactions, oxidation, reduction, and / or other reactions inside the processing system. The gases can be heated to temperatures of 20°C or higher, e.g., 100°C or higher, or 40°C or higher, e.g., 100°C-1000°C, 400°C-900°C, etc., by passing through a suitable heating mechanism, such as an electrically-powered heater, a fuel-fired heater, etc. Alternatively, heating, drying, and / or other reactions inside the processing system can be carried out by directly heating the chamber of the processing system or by directly heating portions of the processing system (e.g., by heating the chamber body of a reaction chamber or a dispersion chamber, etc.).
[0095] The advantages of using heated gas as a heat source include, among others, fast heat transfer, high temperature uniformity, and easy performance enhancement. The reaction chamber can be any chamber, such as a domed ceramic chamber, a quartz chamber, a tubular chamber, or a furnace with an enclosed chamber body. Optionally, the chamber body is made of a thermal insulating material (e.g., ceramic, etc.) to prevent heat loss during drying and / or other reactions within the chamber.
[0096] A gas-liquid mixture formed from one or more gases and one or more liquid droplet streams is delivered to a reaction chamber and undergoes a reaction. The reaction of the gas-liquid mixture in the reaction chamber may include any of oxidation, reduction, decomposition, combination reaction, phase transformation, recrystallization, simple displacement reaction, double displacement reaction, combustion, isomerization, and combinations thereof. For example, one or more gas-liquid mixture streams may be oxidized, e.g., to oxidize liquid mixture compounds to oxide materials. Alternatively, a desired crystal structure of the reaction mixture is obtained from the reaction of one or more gas-liquid mixture streams in the reaction chamber.
[0097] In one embodiment of the present invention, the one or more gases used can be gases that mix thoroughly with the droplet stream to form a gas-liquid mixture, resulting in processing the gas-liquid mixture without reacting with the droplet stream. However, depending on the temperature and chemical composition of the droplet stream, the chemicals in the droplet stream may react to some extent with the gas and / or with each other during processing and / or other reactions inside the chamber. Furthermore, the residence time of the thoroughly mixed gas-liquid mixture of droplet stream compounds inside each of the chambers of the processing system can be adjusted and can range from, for example, 1 second to 1 hour, depending on the flow rate of one or more gases and the path length the droplet stream must travel through the dispersion chamber.
[0098] In one embodiment, the gas-liquid mixture and one or more heated gases can impinge on each other inside the reaction chamber. The gas-liquid mixture stream and the one or more heated gas streams are mixed together to form a reaction mixture inside the reaction chamber over a reaction period, the reaction mixture including the gas stream, the droplet stream, and the heated gas. In another embodiment, the reaction chamber of the processing system can be heated to a reaction temperature T by using one or more gases heated to a temperature between 100° C. and 1400° C. R In one embodiment, one or more heated gases are delivered by a gas delivery element and intermix with one or more gas-liquid mixture streams inside the reaction chamber at an angle (β) between 0 degrees and about 180 degrees.
[0099] Example: Assist gas flow inside the reaction chamber of a processing system Experiments are conducted using a processing system in which gas streams are delivered through a heating assembly into a reaction chamber of the processing system, and the paths of one or more gas streams are tracked and measured.
[0100] FIG. 5 is a cross-sectional view of experimental results showing velocity vectors of one or more heated gases delivered to a processing system. In this example, one or more heated gases, estimated at a temperature of 800° C., are delivered to the processing system through an opening 582 in a reaction chamber wall at a velocity of 13.28 m / s and exit the processing system through a system outlet 584. Multiple vectors 502, 504, 506, 508, 510, 512, 514, 516, 518, 520, and 522, represented by arrows, indicate the direction and magnitude of gas flow at each of the vector locations to simulate heated gas F6. The direction of gas flow at a particular location is indicated by the direction of vectors 502-522, and the magnitude of the gas flow velocity is indicated by the density of vectors 502-522.
[0101] Figure 6 is a cross-sectional view of experimental results showing the distribution of equal velocity lines after one or more heated gases are delivered to a reaction chamber. In this example, a heated gas flow F6, estimated at a temperature of 900°C, is delivered into the reaction chamber through an opening 682 in the chamber wall of the reaction chamber at a velocity of 1 m / s or greater (e.g., about 10 m / s or greater, about 30 m / s or greater, etc.) and is delivered out of the processing system through a system outlet 684. In Figure 6, each line is formed by connecting points having the same velocity, and each of lines 602, 604, 606, 608, 610, 612, 614, 616, 618, 620, 622, and 624 represents a point on the line with the same or equal velocity at the indicated time. The velocity of each line may be 0.1 m / s or greater, and may range from 0.5 m / s to 2.0 m / s, or from 0.1 m / s to 5 m / s, or from 0.1 m / s to 10 m / s. For example, with an input velocity of about 13 m / s, the velocity of each line can range from 8 to 20 m / s. Furthermore, in FIG. 6, the magnitude of lines 602, 604, 606, 608, 610, 612, 614, 616, 618, 620, 622, and 624 indicates an increase in the time of flight of the gas flow that forms a loop inside the reactor chamber and carries the droplets inside the reaction chamber, thereby promoting a chemical reaction process within the reaction chamber, thereby forming uniform particles inside the reaction chamber. For example, the velocity of line 602 and the measured V s1The ratio of the velocity in m / s to the velocity in m / s can be 1:15 to about 1:4. Furthermore, lines 602, 612, 614, 616, and 622 can have the same or similar velocities. The velocity of line 608 and the measured V s1 The ratio of the velocity in m / s to the velocity in m / s can be 1:8 to about 1:3. Furthermore, lines 608 and 610 have the same or similar velocities. The velocity of line 618 and the measured V s1 The ratio of the velocity of the line 624 to the measured V s1 The ratio of velocities in m / s can be from 1:1 to about 1:1.2. Additionally, lines 604, 606, and 624 have the same or similar speeds.
[0102] Figure 7 is a cross-sectional view of experimental results showing the distribution of equal temperature lines after one or more heated gases are delivered to the reaction chamber. In this example, heated gas flow F6, estimated at a temperature of 800°C, is delivered to the reaction chamber through opening 782 at a velocity of 13.28 m / s, and the gas inlet flow rate is 800 CFM (ft 3 / min) and exits the reaction chamber through system outlet 784. In FIG. 7, each line is formed by connecting points having the same speed, and each of lines 702, 704, 706, 708, 710, 712, 714, 716, and 718 represents a point on the line having the same or equal temperature at the indicated time, thereby promoting the formation of uniform particles. The temperatures in FIG. 7 can range from 50°C to 900°C. In FIG. 7, the temperatures at each point in the space between adjacent lines range from 0 to 20°C. The temperature on line 702 represents 720°C, the temperature on line 704 represents 540°C, the temperature on line 706 represents 580°C, the temperature on line 708 represents 600°C, the temperature on line 710 represents 540°C, the temperature on line 712 represents 580°C, the temperature on line 714 represents 600°C, the temperature on line 716 represents 620°C, and the temperature on line 718 represents 640°C.
[0103] Figure 8 is a cross-sectional view of experimental results showing the distribution of equal velocity lines after one or more heated gases are delivered to the reaction chamber. In this example, heated gas flow F6, estimated at a temperature of 800°C, is delivered to the reaction chamber through opening 882 at a velocity of 5.8 m / s, and the gas inlet flow rate is 800 CFM (ft 3 / min) and exits the reaction chamber through system outlet 884. In FIG. 8, each line is formed by connecting points having the same speed, and each of lines 802, 804, 806, 808, 810, 812, 814, and 816 represents a point on the line having the same or equal speed at the time shown, thereby promoting the formation of uniform particles. In FIG. 8, the speeds of lines 802, 804, 806, 808, 810, 812, 814, and 816 form a loop, and all points on the same line have the same speed, and the speed of the line is related to the V measured through opening 882 in the chamber wall of the reaction chamber. s2 The ratio of the velocity in m / s to the velocity in m / s can be 1:200 to about 1:4. For example, lines 802, 804, and 808 have the same or similar velocity. The velocity of line 808 and the measured V s2 The ratio of the velocity of the line 810 to the velocity in m / s can be 1:100 to about 1:40. s2 The ratio of the velocity of the line 814 to the velocity of the line 812 may be 1:60 to about 1:20. Furthermore, the line 810 and the line 812 have the same or similar velocity. s2 The ratio of the velocity of the line 816 to the velocity in m / s can be 1:25 to about 1:10. s2 The ratio of velocity in m / s can be from 1:8 to about 1:4.
[0104] 9 is a cross-sectional view of experimental results showing the distribution of equal temperature lines after one or more heated gases are delivered to the reaction chamber. In this example, heated gas flow F6, estimated at a temperature of 800° C., is delivered to the reaction chamber through opening 982 at a velocity of 5.8 m / s, and the gas inlet flow rate is 350 CFM (ft 3 / min) and exits the reaction chamber through system outlet 984. In FIG. 9, each line is formed by connecting points having the same speed, and each of lines 902, 904, 906, 908, 910, 912, 914, and 916 represents a point on the line having the same or equal temperature at the indicated time, thereby promoting the formation of uniform particles. The temperatures in FIG. 9 can range from 50°C to 900°C. In FIG. 9, the temperatures at each point in the space between adjacent lines range from 0°C to 12°C. The temperature of line 902 represents 680°C, the temperature of line 904 represents 620°C, the temperature of line 906 represents 560°C, the temperature of line 908 represents 560°C, the temperature of line 910 represents 584°C, the temperature of line 912 represents 584°C, and the temperature of line 914 represents 620°C.
[0105] The foregoing is directed to embodiments of the present invention; other and further embodiments of the invention may be devised without departing from the basic scope thereof, which scope is determined by the claims that follow.
Claims
1. 1. A method of producing a product from a liquid mixture by a heating assembly in a processing system, comprising: delivering one or more first gas streams to a system inlet via a first gas line; forming a liquid mixture, the liquid mixture comprising a lithium-containing compound and one or more metal-containing compounds; ejecting the liquid mixture into one or more droplet streams by one or more power jet modules into the processing system; dispersing the one or more droplet streams into the one or more first gas streams to form one or more gas-liquid mixtures in a dispersion chamber connected to the one or more power jet modules and adapted to disperse the one or more droplet streams with the one or more first gas streams to form one or more gas-liquid mixtures; delivering one or more second gas streams to a reaction chamber of the processing system via a heating assembly, the reaction chamber being connected to a distribution chamber, the heating assembly comprising: a second gas line connected to an opening in a chamber wall of the reaction chamber for delivering one or more second gas streams to the reaction chamber; a gas delivery element connected to the second gas line and positioned inside the reaction chamber, the gas delivery element extending to an inlet region of the reaction chamber and positioned upwardly within the reaction chamber to deliver the one or more second gas streams to the inlet region, the inlet region being connected to a dispersion chamber, into the interior of the reaction chamber through which the one or more second gas streams are delivered, forming a reaction mixture with the one or more gas-liquid mixtures; treating the reaction mixture in the reaction chamber to produce a product comprising a lithium-containing compound and one or more metal-containing compounds.
2. The method of claim 1 , wherein the one or more first gas streams and the one or more droplet streams flow relative to one another at a divergence angle (α) between 0 and 180 degrees.
3. The method of claim 1 , wherein the gas delivery element is positioned inside the reaction chamber and extends to an inlet region of the reaction chamber, the inlet region being connected to the distribution chamber of the processing system.
4. 10. The method of claim 1, wherein the one or more second gas streams are delivered by the gas delivery element and intermix with one or more gas-liquid mixture streams inside the reaction chamber at an angle (β) between 0 and 180 degrees.
5. 5. The method of claim 4, wherein the angle (β) is 180 degrees.
6. 10. The method of claim 1, wherein the lithium-containing compound is a material selected from the group consisting of lithium-containing compounds, lithium sulfate (LiSO), lithium nitrate (LiNO), lithium carbonate (LiCO), lithium acetate (LiCHCOO), lithium hydroxide (LiOH), lithium formate (LiCHO), and lithium chloride (LiCl).
7. The one or more metal-containing compounds may be a manganese-containing compound, a nickel-containing compound, a cobalt-containing compound, cobalt sulfate (CoSO4), cobalt nitrate (Co(NO3)2), cobalt carbonate (CoCO3), cobalt acetate (Co(CH2COO)2), cobalt hydroxide (Co(OH)2), cobalt formate (Co(CHO2)2), cobalt chloride (CoCl2), manganese sulfate (MnSO4), manganese nitrate (Mn(NO3)2), manganese carbonate (MnCO3), manganese acetate (Mn(CH2COO)2), manganese hydroxide (Mn(OH)2), manganese formate (Mn(CHO2)2), manganese chloride (MnCl2), nickel sulfate (NiSO4), nitric acid 10. The method of claim 1, wherein the nickel-containing compound is a material selected from the group consisting of nickel (Ni(NO3)2), nickel carbonate (NiCO3), nickel acetate (Ni(CH2COO)2), nickel hydroxide (Ni(OH)2), nickel formate (Ni(CHO2)2), nickel chloride (NiCl2), aluminum (Al)-containing compounds, titanium (Ti)-containing compounds, sodium (Na)-containing compounds, potassium (K)-containing compounds, rubidium (Rb)-containing compounds, vanadium (V)-containing compounds, cesium (Cs)-containing compounds, chromium (Cr)-containing compounds, copper (Cu)-containing compounds, magnesium (Mg)-containing compounds, iron (Fe)-containing compounds, or combinations thereof.
8. The method of claim 1 , wherein the processing system further comprises an electronic control center.
9. 10. The method of claim 1, wherein the one or more first gas streams delivered through one or more first gas lines are maintained at a first temperature and the one or more second gas streams delivered through the gas delivery elements of the heating assembly are maintained at a second temperature, the second temperature being higher than the first temperature.
10. 10. The method of claim 9, wherein the first temperature is maintained at a temperature between 20°C and 400°C.
11. 10. The method of claim 9, wherein the second temperature is maintained at a temperature between 100°C and 1400°C.
12. 2. The method of claim 1, wherein the gas mixture comprises a lithium-containing salt and a cobalt-containing salt, and the lithium-containing salt and the cobalt-containing salt can be dissolved in a suitable solvent, and the suitable solvent is selected from the group consisting of water, alcohol, methanol, isopropyl alcohol, an organic solvent, an inorganic solvent, and combinations thereof.
13. 10. The method of claim 1, wherein the product is a lithium metal oxide.
14. 1. A method of producing a product from a liquid mixture by a heating assembly in a processing system, comprising: delivering one or more first gas streams to a system inlet via a first gas line; forming a liquid mixture, the liquid mixture comprising a lithium-containing compound and one or more metal-containing compounds; ejecting the liquid mixture into one or more droplet streams by one or more power jet modules into the processing system; dispersing the one or more droplet streams into the one or more first gas streams to form one or more gas-liquid mixtures; delivering one or more second gas flows to a reaction chamber of the processing system via a heating assembly, the heating assembly comprising: a second gas line connected to an opening in a chamber wall of the reaction chamber for delivering one or more second gas streams to the reaction chamber; a gas delivery element connected to the second gas line and positioned inside the reaction chamber, the gas delivery element extending to an inlet region of the reaction chamber and positioned upwardly within the reaction chamber to deliver the one or more second gas streams to the inlet region, the inlet region being connected to a dispersion chamber, into the interior of the reaction chamber through which the one or more second gas streams are delivered, forming a reaction mixture with the one or more gas-liquid mixtures; treating the reaction mixture in the reaction chamber to produce a product comprising a lithium-containing compound and one or more metal-containing compounds; The method of claim 1, wherein the one or more second gas streams are delivered by the gas delivery element and intermix with one or more gas-liquid mixture streams at an angle (β) of 180 degrees inside the reaction chamber.
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