High temperature sintering furnace system and method

Abstract

A sintering furnace can have a housing, one or more heating elements, and a transport assembly. Each heating element can be disposed within the housing and can subject a heating zone to a thermal shock temperature profile. Through the transport assembly, a substrate having one or more precursors thereon can be moved through an inlet of the housing to the heating zone, where the substrate is at a first temperature of at least 500 °C for a first period of time. The transport assembly can then move the substrate having one or more sintered materials thereon from the heating zone and from an outlet of the housing.

Description

[0001] Cross-references to related applications

[0002] This application claims the benefit of U.S. Provisional Patent Application No. 63 / 166,941, filed March 26, 2021, entitled “High Temperature Sintering Furnace System,” the entire contents of which are incorporated herein by reference.

[0003] Statement on Federally Funded Research

[0004] This invention was granted government funding under designation DEAR0001329 by the Department of Energy's (DOE) Advanced Research Projects Agency for Energy (ARPA-E). The government owns certain rights to this invention. Technical Field

[0005] The present invention generally relates to furnaces for heating materials, and more specifically, to high-temperature (e.g., ≥500°C) furnace systems and methods for sintering materials. Background Technology

[0006] High-temperature sintering can be used to process ceramic materials, for example, in electronic environments, energy storage environments, and extreme environments. Traditional sintering techniques, such as tube furnaces or muffle furnaces, typically require long sintering times (e.g., 10 hours), mild temperatures (approximately 1300 K), slow heating rates (e.g., 10 K / min), and high energy input. Furthermore, traditional sintering techniques may introduce voids or contaminants into sintered materials containing volatile elements (e.g., Na, Li, etc.). These defects can render sintered products unsuitable for certain applications, such as ceramic-based solid electrolytes (SSEs). Additionally, traditional sintering techniques may have limited control over the crystal coarsening process, where abnormal grain growth and inconsistent size distributions can cause problems.

[0007] While faster sintering techniques such as microwave-assisted sintering (MAS), spark plasma sintering (SPS), and flash sintering (FS) have recently been developed, they each have their own problems or limited applications. For example, MAS often depends on the microwave absorption properties of the material or the use of absorbents. SPS, also known as field-assisted sintering (FAST) or pulsed current sintering (PECS), can produce dense ceramics at moderate pressures within relatively short sintering times (e.g., 2 to 10 minutes) and low temperature ranges (e.g., 1073 to 1883 K). However, SPS requires complex and expensive equipment to simultaneously provide mechanical pressure (e.g., 6 to 100 MPa) and high-pulse DC current (e.g., up to several thousand amperes). While FS does not require complex instrumentation, it requires expensive platinum electrodes, and the conditions required to perform FS depend on the electrical properties of the material (and may therefore be limited to certain materials). MAS, SPS, and FS systems are difficult to integrate into roll-to-roll processing systems, which may hinder their ability to provide large-scale manufacturing capabilities.

[0008] Embodiments of the disclosed subject matter can solve one or more of the above-described problems and defects. Summary of the Invention

[0009] Embodiments of the disclosed subject matter provide high-temperature sintering furnace systems and methods. In some embodiments, the high-temperature sintering furnace system may include a roll-to-roll processing configuration, which enables large-scale and / or continuous manufacturing of sintered materials (e.g., ceramics). The sintering furnace may have one or more heating elements (e.g., Joule heating elements) that generate sintering temperatures exceeding 500°C (e.g., about 1000-3000°C) within a relatively short time (e.g., ≤60 s, e.g., ≤ about 10 s). In some embodiments, each heating element can be rapidly heated to and / or rapidly cooled from the sintering temperature. For example, the heating elements may be heated at at least 10 3 Heating rate of ℃ / min (e.g., ≥10) 3 ℃ / s, for example 10 3 -10 4 The temperature transitions from a low temperature (e.g., room temperature, such as 20-25°C, or a high temperature far below 500°C, such as 200°C) to the sintering temperature (°C / s (inclusive)). Alternatively or additionally, in some embodiments, the heating element may be at least 10 °C / s. 4 ℃ / min (e.g., ≥10) 4 The cooling rate (℃ / s) transitions from the sintering temperature to a lower temperature (e.g., room temperature or a high temperature below 500℃, such as 200℃).

[0010] In one or more embodiments, the sintering furnace may include a shell, at least one heating element, a transfer assembly, and a control system. The shell may define an internal volume, an inlet to the internal volume, and an outlet to the internal volume. At least one heating element may be disposed within the internal volume of the shell and located between the inlet and the outlet. Each heating element may be configured to subject a heating region to a temperature profile. The transfer assembly may be configured to move one or more substrates into, within, and out of the shell. The control system may be operatively coupled to at least one heating element and the transfer assembly. The control system may include one or more processors and a computer-readable storage medium storing instructions that, when executed by the one or more processors, cause the control system to move a first substrate having one or more precursors thereon through the inlet to the heating region via the transfer assembly; subject the first substrate in the heating region to a first temperature of at least 500°C for a first time period via the at least one heating element; and remove the first substrate having one or more sintered materials thereon through the outlet from the heating region via the transfer assembly.

[0011] In one or more embodiments, the sintering furnace may include a shell, a distributor, at least one heating element, a sampler, and a control system. The shell may define an internal volume, an inlet to the internal volume, and an outlet to the internal volume. The distributor may be configured to provide one or more precursor particles to the inlet of the shell; the at least one heating element may be disposed within the internal volume of the shell and located between the inlet and the outlet. Each heating element may be configured to subject one or more precursor particles to a temperature profile. The sampler may be configured to receive one or more sintered particles from the outlet of the shell. The control system may be operatively coupled to the at least one heating element. The control system may include a computer-readable storage medium storing instructions for one or more processors, which, when executed by the one or more processors, cause the control system to subject one or more precursor particles to a first temperature of at least 500°C for a first time period via the at least one heating element.

[0012] Any of the various innovations disclosed herein can be used in combination or alone. The present invention provides a simplified version of some concepts, which will be further elaborated in the detailed description below. This present invention is not intended to identify key or essential features of the claimed subject matter, nor is it intended to limit the scope of the claimed subject matter. The foregoing and other objects, features, and advantages of the disclosed technology will become more apparent from the following detailed description with reference to the accompanying drawings. Attached Figure Description

[0013] The embodiments will now be described with reference to the accompanying drawings, which are not necessarily drawn to scale. Where applicable, some elements may be simplified or otherwise omitted to aid in the illustration and description of essential features. Throughout the drawings, the same reference numerals denote the same elements.

[0014] Figure 1A It is a simplified cross-sectional view of a high-temperature sintering furnace according to one or more embodiments of the disclosed subject matter.

[0015] Figure 1B This is a simplified cross-sectional view of a roll-to-roll processing system using a high-temperature sintering furnace according to one or more embodiments of the disclosed subject matter.

[0016] Figure 1C It is a simplified cross-sectional view of another high-temperature sintering furnace employing a single inlet and outlet, according to one or more embodiments of the disclosed subject matter.

[0017] Figure 2 It describes general examples of computing environments in which the disclosed techniques can be implemented.

[0018] Figure 3A It is a graph showing an exemplary temperature distribution of the heating element of a high-temperature sintering furnace according to one or more embodiments of the disclosed subject matter.

[0019] Figure 3B It is an exemplary multi-temperature graph of a substrate carrying a material to be sintered, according to one or more embodiments of the disclosed subject matter.

[0020] Figure 4A This is a simplified perspective view of a heating element for a high-temperature sintering furnace according to one or more embodiments of the disclosed subject matter.

[0021] Figures 4B to 4C These are simplified cross-sectional views and partial perspective views of a heating element with exemplary electrical connections for a high-temperature sintering furnace according to one or more embodiments of the disclosed subject matter.

[0022] Figure 5A This is a simplified cross-sectional view of an exemplary two-stage heating system employing a single furnace, according to one or more embodiments of the disclosed subject matter.

[0023] Figure 5B This is a simplified cross-sectional view of an exemplary two-stage heating system employing a separate furnace, according to one or more embodiments of the disclosed subject matter.

[0024] Figure 6 This is a simplified cross-sectional view of an exemplary batch processing system employing multiple heating elements in a single furnace, according to one or more embodiments of the disclosed subject matter.

[0025] Figures 7A to 7B This is a simplified cross-sectional view of an exemplary high-temperature sintering furnace with active cooling of the outer surface, according to one or more embodiments of the disclosed subject matter.

[0026] Figures 8A to 8B The following is a simplified perspective view and cross-sectional view of a heating element having a nozzle for protecting airflow, according to one or more embodiments of the disclosed subject matter.

[0027] Figure 8C This is a simplified cross-sectional view of a high-temperature sintering furnace having an integrated nozzle for protecting the airflow, according to one or more embodiments of the disclosed subject matter.

[0028] Figure 9 These are a series of simplified cross-sectional views, based on one or more embodiments of the disclosed subject matter, illustrating the operation of an exemplary high-temperature sintering furnace employing heating and pressing.

[0029] Figure 10 This is a simplified cross-sectional view of an exemplary high-temperature sintering furnace that employs a portion of a conveyor belt as a heating element according to one or more embodiments of the disclosed subject matter.

[0030] Figure 11A This is a simplified perspective view of a portion of an exemplary high-temperature sintering furnace according to one or more embodiments of the disclosed subject matter, the exemplary high-temperature sintering furnace employing a pair of opposing heating elements and a substrate for conveying.

[0031] Figure 11B It is shown Figure 11A A series of simplified cross-sectional diagrams of the operation of the high-temperature sintering furnace.

[0032] Figures 12A to 12B These are simplified cross-sectional and perspective views of a portion of an exemplary high-temperature sintering furnace according to one or more embodiments of the disclosed subject matter, the exemplary high-temperature sintering furnace employing a pair of opposing heating elements, material compression, and material transfer.

[0033] Figures 13A to 13B The figures are simplified cross-sectional and perspective views of a portion of an exemplary high-temperature sintering furnace employing a pair of opposing heating elements, according to one or more embodiments of the disclosed subject matter, wherein the exemplary high-temperature sintering furnace has no material transfer.

[0034] Figures 14A to 14B The figures are simplified cross-sectional and perspective views of a portion of an exemplary high-temperature sintering furnace employing a pair of opposing heating elements according to one or more embodiments of the disclosed subject matter, the sintering furnace having a material compression function but no material transport.

[0035] Figures 15A to 15CThese are simplified outlet side view, perspective view, and partial perspective view of an exemplary high-temperature sintering furnace employing active external cooling, according to one or more embodiments of the disclosed subject matter.

[0036] Figures 16A to 16C These are simplified cross-sectional views, perspective views, and partial perspective views of exemplary high-temperature sintering furnaces employing internal insulation materials and protective airflow according to one or more embodiments of the disclosed subject matter.

[0037] Figures 17A to 17B These are simplified cross-sectional views of the internal volumes of an exemplary high-temperature sintering furnace employing active cooling and an exemplary high-temperature sintering furnace employing insulating materials, respectively, according to one or more embodiments of the disclosed subject matter.

[0038] Figures 18A to 18B These are simplified cross-sectional and perspective views of a portion of a high-temperature sintering furnace employing one or more shells for protecting the gas flow, according to one or more embodiments of the disclosed subject matter.

[0039] Figure 19A This is a simplified perspective view of a portion of an exemplary high-temperature sintering furnace according to one or more embodiments of the disclosed subject matter, the exemplary high-temperature sintering furnace employing mechanical loading / unloading of material and a single pair of heating elements.

[0040] Figure 19B This is a simplified perspective view of a portion of another exemplary high-temperature sintering furnace according to one or more embodiments of the disclosed subject matter, the exemplary high-temperature sintering furnace employing mechanical loading / unloading of material and multiple pairs of heating elements.

[0041] Figure 20 This is a simplified perspective view of a portion of an exemplary high-temperature sintering furnace according to one or more embodiments of the disclosed subject matter, the exemplary high-temperature sintering furnace employing precursor particles dispensed on a conveyor belt.

[0042] Figure 21A This is a simplified cross-sectional view of a portion of an exemplary gas-supported flow-through high-temperature sintering furnace according to one or more embodiments of the disclosed subject matter.

[0043] Figure 21B It is applicable to one or more embodiments of the disclosed subject matter. Figure 21A A simplified plan view of an exemplary flow-through heating element in a sintering furnace.

[0044] Figure 22 It is a simplified perspective view of a portion of an exemplary gravity-guided flow through a high-temperature sintering furnace according to one or more embodiments of the disclosed subject matter. Detailed Implementation

[0045] Overview

[0046] For ease of explanation, this document will describe certain aspects, advantages, and novel features of embodiments of this disclosure. The disclosed methods and systems should not be construed as limiting in any way. Rather, this disclosure is directed to all novel and non-obvious features and aspects of the various embodiments disclosed, whether individually or in various combinations and sub-combinations. These methods and systems are not limited to any particular aspect or feature or combination thereof, and the disclosed embodiments do not claim to possess any one or more particular advantages or problems solved. The techniques in any embodiment or example can be combined with the techniques described in any one or more other embodiments or examples. Given that the principles of the disclosed technology can be applied to many possible embodiments, it should be understood that the illustrated embodiments are merely exemplary and should not be considered as limiting the scope of the disclosed technology.

[0047] Although the operations of some of the disclosed methods are described in a specific order for ease of description, it should be understood that this descriptive approach includes rearrangement unless the specific language below requires a particular order. For example, operations described in sequence may be rearranged or performed simultaneously in certain situations. Furthermore, for simplicity, the accompanying drawings may not show various ways in which the disclosed methods are used in combination with other methods. Additionally, the specification sometimes uses terms such as “provide” or “implementation” to describe the disclosed methods. These terms represent high-level abstractions of the actual operations performed. The actual operations corresponding to these terms may vary depending on the specific implementation and are readily discernible to those skilled in the art.

[0048] Unless otherwise stated, the disclosure of numerical ranges should be understood to refer to each discrete point within the range, including the endpoints. Unless otherwise stated, all figures used in the specification or claims indicating component quantities, molecular weights, percentages, temperatures, times, etc., should be understood to be modified by the term "about". Therefore, unless otherwise implied or explicitly stated, or unless a person skilled in the art has a clearer understanding of the context, the numerical parameters listed are approximate values ​​that may depend on the desired characteristics and / or detection limits under standard test conditions / methods well known to those skilled in the art. When directly and explicitly distinguishing embodiments from the prior art discussed, embodiment numbers are not approximate values ​​unless the word "about" is used. Unless otherwise explicitly stated, whenever "substantially," "approximately," "about," or similar wording is explicitly used in conjunction with a particular value, it means that the variation may be as high as 10% (inclusive) of that value.

[0049] Orientation and other relative references are used to facilitate discussion of the figures and principles herein, but are not intended to be limiting. For example, terms such as “inner,” “outer,” “upper,” “lower,” “top,” “bottom,” “internal,” “external,” “left,” “right,” “front,” “rear,” and “rear” may be used. These terms (where applicable) are used to make the description clearer when dealing with relative relationships, particularly with respect to the illustrated embodiments. However, these terms do not imply absolute relationships, positions, and / or orientations. For example, for an object, simply flipping it over will turn the “upper” portion into the “lower” portion. Nevertheless, it remains the same portion, and the object remains the same.

[0050] As used herein, “comprising” means “including”, and the singular forms “a” or “an” or “the” include the plural, unless the context clearly specifies otherwise. The term “or” refers to a single element or a combination of two or more elements among the elucidated alternative elements, unless the context clearly specifies otherwise.

[0051] While alternatives exist for the various components, parameters, and operating conditions described herein, this does not imply that these alternatives are necessarily equivalent and / or perform as well. Unless otherwise stated, the alternatives are not listed in order of priority. Unless otherwise stated, any combination defined below may be either substituted or not substituted.

[0052] Unless otherwise stated, all 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 pertains. While similar or equivalent methods and materials to those described herein may be used in the practice or testing of this disclosure, suitable methods and materials will be described below. Materials, methods, and examples are illustrative only and not restrictive. The features of the subject matter of this disclosure will become apparent from the following detailed description and the appended claims.

[0053] Terminology Overview

[0054] The following are explanations of specific terms and abbreviations to facilitate the description of various aspects of the disclosed subject matter and to guide those skilled in the art in practicing the disclosed subject matter.

[0055] Thermal shock: The duration of application of the sintering temperature is less than about 10 seconds. In some embodiments, the duration of application of the sintering temperature is in the range of about 1 microsecond to about 10 seconds (e.g., including about 55 milliseconds).

[0056] Sintering temperature: The highest temperature on the surface of the heating element when it is energized (e.g., by applying a current pulse). In some embodiments, the sintering temperature is at least 500°C, for example, in the range of 1000-3000°C. In some embodiments, the temperature of the material sintered in the furnace may match or substantially match the temperature of the heating element (e.g., within 10%).

[0057] Inert gases: gases that do not undergo chemical reactions at the sintering temperature. In some embodiments, inert gases are nitrogen, argon, helium, neon, krypton, xenon, radon, etc. Or any combination thereof.

[0058] Refractory material: A material (e.g., an element or compound) with a melting temperature of at least 1000°C (e.g., at least 1580°C). In some embodiments, the refractory material may be a refractory material as defined in ASTM C71-01 "Standard Terminology Relating to Refractories" (August 2017), which is incorporated herein by reference.

[0059] Refractory metal: a metal or metal alloy with a melting point of at least 1000°C (e.g., at least 1850°C). In some embodiments, the refractory metal is one of niobium, molybdenum, tantalum, tungsten, rhenium, or an alloy thereof.

[0060] Metals: include individual chemical elements that are classified as metals in the periodic table, including alkali metals, alkaline earth metals, transition metals, lanthanides and actinides, as well as alloys formed from these metals (e.g., but not limited to stainless steel, brass, bronze, Monel alloys, etc.).

[0061] introduce

[0062] Figure 1A An exemplary high-temperature sintering furnace system 100 is illustrated. The sintering furnace system 100 may have a housing 108, which includes and / or defines an inlet 110, an outlet 112, and an internal volume 114 disposed along the direction of travel between the inlet 110 and the outlet 112. In some embodiments, the inner surface of the housing 108 defining the volume 114 may be formed or coated with one or more low-emissivity materials (e.g., gold, chromium, zinc, copper, silver, aluminum, silicon, lead, etc.), which can help improve the efficiency of the furnace 100. The inlet 110 may be defined with a height of t. i The opening (e.g., in a direction perpendicular to the direction of travel) can be defined with a height of t. o The opening (e.g., in a direction perpendicular to the direction of travel). In some embodiments, the entrance height t i and / or exit height t oThe size can be selected to be as small as possible, while still allowing the material to be sintered to enter without contacting the inlet 110, and the sintered material to exit without contacting the outlet 112.

[0063] Heating element 116 may be disposed within the internal volume 114 of housing 108, located between inlet 110 and outlet 112 (e.g., substantially midway between inlet and outlet along the direction of travel). Heating element 116 may subject heating region 124 to a thermal shock profile, for example, as will be described below. Figures 3A to 3B Further details are provided. In some embodiments, the heating element is a Joule heating element, for example, formed of carbon, graphite, metal, or any combination thereof. Electrical contact between the power source 118 (e.g., a current source, such as a waveform generator) and the heating element 116 can be achieved by lines extending through respective feedlines or passages 120a, 120b (e.g., formed of refractory material). The controller 122 is operatively coupled to the current source 118 to control the operation of the current source 118, for example, controlling the current source 118 to apply current pulses to the heating element 116, subjecting the heated region 124 to a thermal shock profile. In some embodiments, the heating element may include any other heating source capable of generating a thermal shock profile, such as a microwave heating source, a laser, an electron beam device, a spark discharge device, or any combination thereof, in place of or as a supplement to Joule heating.

[0064] exist Figure 1A In the example shown, a gap g (e.g., the minimum distance between the heating element 116 and the material to be sintered in the heating zone 124 in a direction perpendicular to the material travel direction) is provided between the heating element 116 and the material to be sintered and / or the top surface of the sintered material to provide radiant heating. Alternatively or additionally, the heating element 116 may be moved to contact the material to be sintered to provide conductive heating. For example, an actuator (e.g., such as...) may be provided. Figure 9 (As shown) to move the heating element 116 toward the material to be sintered (e.g., reducing the gap g to zero) for thermal shock heating, and then move it away from the sintered material (e.g., increasing the gap g to a safe distance) to convey the material out of the housing. Although Figure 1A The example shown only illustrates a single heating element 116, but embodiments of the disclosed subject matter are not limited thereto. Rather, for example, multiple heating elements may be provided, according to one or more contemplated embodiments, to provide series heating (e.g., by placing the heating elements at different locations along the direction of travel through the housing 108) and / or parallel heating (e.g., by placing the heating elements on opposite sides of the material to be sintered).

[0065] exist Figure 1AIn the illustrated example, the internal volume 114 is substantially open; for example, there is a considerable distance between the inner wall of the housing 108 defining the internal volume 114 and the component passing through the housing 108 (e.g., conveyor belt 102). For example, in some embodiments, the size of the internal volume 114 may be at least an order of magnitude larger (e.g., at least 10 times, for example, at least 100 times) than the volume of the heating region 124 (e.g., the region within 10% of the sintering temperature during thermal shock). Alternatively or additionally, in some embodiments, the size of the internal volume 114 may be at least 10 times larger than the volume of the heating element. 7 For example, a carbon-based Joule heater (e.g., with dimensions of approximately 10cm × 1cm × 0.2cm) maintaining a temperature of approximately 3000°C in a stainless steel cavity or shell might require approximately 15kW of electrical power. Without furnace cooling or insulation, if the shell dimensions are approximately 1.87m × 1.87m × 1.87m (equivalent to 3.4 × 10⁻⁶), the required power would be significantly higher. 6 (Based on the volume ratio), the temperature of the outer wall of the shell can reach approximately 200°C. In contrast, if the size of the cavity is increased to approximately 2.8m × 2.8m × 2.8m (equivalent to approximately 1.0 × 10⁻⁶ m), the temperature of the outer wall can reach approximately 200°C. 7 (by volume ratio), the temperature of the outer wall of the shell can be maintained at about 100°C.

[0066] Alternatively or additionally, the travel length L of the furnace shell 108 between the inlet 110 and the outlet 112 行进 It can be at least longer than the heating area 124 by length L HZ This is an order of magnitude larger (e.g., at least 10 times, or at least 100 times). This configuration facilitates rapid cooling of the heating element 116 at the end of the thermal shock curve (e.g., and rapid cooling of the accompanying sintered material). Alternatively or additionally, in some embodiments, the size of the internal volume 114 can be reduced, for example, by means of thermal insulation material disposed between the heating region 124 and the walls of the housing 108. This thermal insulation material helps prevent the high temperatures reached during thermal shock from being transferred to the outer surface of the housing 108 and / or the surrounding environment.

[0067] A transfer assembly can be used to move the material to be sintered into the internal volume 114 of the housing 108 via inlet 110 and to remove the sintered material from the internal volume 114 of the housing 108 via outlet 112. For example, in some embodiments, the transfer assembly may include a conveyor belt 102 (e.g., a continuous conveyor belt), one or more drive rollers 104a, 104b (e.g., including or coupled to a rotary motor), and one or more support rollers 106a, 106b (e.g., passive rollers). In the illustrated example, the drive rollers 104a, 104b are held outside the housing 108 and are therefore isolated from the high temperatures generated within the housing 108 during thermal shock. Because the support rollers 106a, 106b are disposed within the housing 108, they can be formed of a refractory metal (e.g., tungsten). Alternatively, if the support rollers 106a, 106b are sufficiently spaced from the heating zone 124, they can be formed of a non-refractory metal (e.g., stainless steel).

[0068] The conveyor belt 102 may be formed of a flexible material capable of withstanding one or more applied sintering temperatures. For example, in some embodiments, the conveyor belt 102 may be formed of a carbon-based material (e.g., graphite). Alternatively, in some embodiments, the conveyor belt 102 may be formed of a material that cannot withstand the sintering temperatures (e.g., due to melting, carbonization, or other degradation effects). For example, in some embodiments, the conveyor belt may be formed of a polymer fabric. In this case, the material to be sintered can be conveyed from the conveyor belt to a high-temperature support (not shown) or heating element surface within the heating zone, and any sintered material can be conveyed back to the conveyor belt for transfer from the internal volume 114 (e.g., from the heating zone 124).

[0069] In operation, the material 128i to be sintered can be conveyed into the housing 108 via inlet 110, and the sintered material 128s can be conveyed out of the housing 108 via outlet 112. In some embodiments, the material 128i to be sintered may include nanoparticles and / or precursors (e.g., metal salts, such as chlorides or hydrates of elemental metals). Alternatively or additionally, the material 128i to be sintered may be disposed on a substrate, such as a polymer film (e.g., green tape). In some embodiments, the combination of the material 128i to be sintered (and any substrate) with the conveyor belt 102 can have a maximum thickness t. m The maximum thickness t m Slightly smaller than the inlet thickness t i and / or outlet thickness t o For example, the inlet thickness t i Export thickness t o Or the two can be compared in terms of thickness t mThe inlet thickness is at least 10% greater, which helps prevent the surrounding environment of housing 108 from being exposed to the high temperatures inside housing 108. Alternatively or additionally, in some embodiments, the inlet thickness t i Export thickness t o Or both can not exceed the thickness t m Twice as much.

[0070] Despite Figure 1A The specific configuration of the transmission components is shown, but other configurations are possible according to one or more contemplated embodiments. For example, one or both of the support rollers 106a and 106b may be omitted, or additional support rollers may be provided inside or outside the housing 108. In another example, one or more drive rollers may be provided inside the housing 108 in addition to or in place of drive rollers 104a and 104b. Furthermore, although in Figure 1A In the example, a continuous conveyor belt 102 is used, but in some embodiments, the transport components may alternatively employ a roller-to-roll processing configuration.

[0071] For example, Figure 1B An exemplary sintering furnace system 130 with a roll-to-roll configuration is shown, wherein a supply roll 132 unfolds to feed conveyor material 136 to an inlet 110, and the processed conveyor material 136 from an outlet 112 is wound onto an output roll 134. In some embodiments, the conveyor material 136 may include the material to be sintered (e.g., one or more precursors, for example, in the form of a substantially solid). Alternatively or additionally, the conveyor material 136 may be used as a support for the material to be sintered thereon, for example, by preloading one or more precursors onto at least one surface of the conveyor material 136 and winding it around the supply roll 132, wherein once supplied to the heating zone, the at least one surface will face the heating element 116. Alternatively or additionally, the conveyor material 136 may support the material to be sintered therein, for example, by having one or more precursors (e.g., nanoparticles) on fibers (e.g., carbon nanofibers) forming the conveyor material.

[0072] exist Figures 1A to 1B In one example, housing 108 has an inlet 110 separated from outlet 112, and a conveyor belt or material extends through the internal volume 114 between inlet 110 and outlet 112. However, in other embodiments, a single port can be used to supply material to the heating zone and remove sintered material from the heating zone. This single-port configuration can improve system efficiency, for example, by minimizing openings to reduce heat loss from the internal volume of the housing and / or the entry of impurities from the outside of the housing into the internal volume.

[0073] For example, Figure 1CAn exemplary single-port sintering furnace system is illustrated in loading / unloading stage 140 and sintering stage 152. Similar to the example above, housing 150 defines an internal volume 146 providing heating element 116. However, housing 150 includes a single inlet / outlet 148 through which material is introduced and then removed from internal volume 146. Material 128i to be sintered may be disposed on material support member 142 (e.g., a rigid substrate), which may be laterally moved via actuation assembly 144 through inlet / outlet 148 to position material 128i for sintering, as shown in sintering stage 152. In the illustrated example, actuation assembly 144 employs a pair of rollers that rotate about an axis perpendicular to the drawing. Alternatively, in some embodiments, actuation of the actuation assembly employs a rotary table, in which actuation causes member 142 to rotate about an axis parallel to the drawing (e.g., an axis parallel to the gap g between the heating element and the material in the heating region).

[0074] In any disclosed example, the heating element can subject the material in the heating region to a thermal shock profile. For example, controller 122 can control power supply 118 to apply a short-duration current pulse to heating element 116, causing the heating element to rapidly heat up to the sintering temperature, remain at the sintering temperature for a predetermined sintering time, and then rapidly cool down from the sintering temperature. For example, Figure 3A A temperature profile 300, which can be generated by a heating element, is shown to perform a thermal shock process. During the first sintering stage 302a, a sintering temperature T can be provided for a relatively short time period t1 (e.g., less than or equal to 60 s, for example, in the range of about 1 μs to 10 s (inclusive), for example, about 10 s). H (For example, at least 500°C, for example, in the range of 1000-3000°C (inclusive), for example, about 2000°C or higher). In some embodiments, the high temperature is sufficient to melt all constituent precursor materials and / or sufficient to initiate high-temperature homogeneous mixing. In some embodiments, the temperature profile 300 can provide up to the sintering temperature T. H And / or from the sintering temperature T H A rapid transition. For example, a temperature profile of 300 can exhibit a transition of at least 10. 2 Heating slope R at ℃ / s H (For example, from the base temperature T) L (e.g., room temperature (e.g., 20-25℃) or higher ambient temperature (e.g., 100-200℃)) raise to sintering temperature T H ), for example 10 3 -10 4 ℃ / s (inclusive). The temperature curve 300 can also show at least 10. 2 Cooling slope R at ℃ / s C (For example, from the sintering temperature T)H to base temperature T L And / or from the sintering temperature T H (to the melting temperature of one or more of the precursor's constituent materials), for example, 10 3 -10 4 °C / s (inclusive). For example, systems and methods for thermal shock may be similar to U.S. Patent Publication No. 2018 / 0369771 entitled "Nanoparticles and systems and methods for synthesizing nanoparticles through thermal shock", U.S. Patent Publication No. 2019 / 0161840 entitled "Thermal shock synthesis of multielement nanoparticles", International Publication No. WO2020 / 236767 entitled "High temperature sintering systems and methods", and International Publication No. WO2020 / 252435 entitled "Systems and methods for high temperature synthesis of single atom dispersions and multi-atom dispersions", all of which are incorporated herein by reference.

[0075] In some embodiments, thermal shock exposure may be performed in batches, for example, by feeding material into a heated zone, keeping it substantially stationary during exposure to the sintering temperature, and then feeding it out of the heated zone during or after cooling. In such embodiments, temperature profile 300 may include a subsequent sintering stage 302b, which may be substantially the same as the first sintering stage 302a, but time-delayed by t2. In some embodiments, delay t2 may be equal to or greater than the time period for removing sintered material (or a group thereof) from the heated zone and / or introducing the next material (or a group thereof) to be sintered into the heated zone. In some embodiments, t2 may be less than the sintering time period t1 (e.g., at least an order of magnitude smaller than t1). Alternatively or additionally, t2 may be substantially equal to or greater than t1.

[0076] Alternatively, in some embodiments, thermal shock exposure can be performed continuously, for example, by conveying material to and through the heating zone while the heating element provides a thermal shock profile. In such embodiments, the passage time through the heating zone and the thermal shock profile can be coordinated to ensure that the cumulative amount of time each type of material is exposed to the sintering temperature through the heating zone is substantially equal to the required sintering time (e.g., less than a predetermined maximum time). Alternatively or additionally, thermal shock exposure can be generated at least in part by the transport of material through the heating zone (e.g., t1 = L). HZ ÷(the speed at which the material travels through the heated zone)).

[0077] In some embodiments, the material to be sintered may be pre-temperature profiled before thermal shock profiling, for example, to prepare precursor materials and / or a substrate supporting the precursor materials for subsequent thermal shock. Figure 3B The multi-stage temperature profile 310 of the material to be sintered is shown. During the preheating stage 312, the material can be at an intermediate temperature T. I The duration is t3. In some embodiments, the preheating stage 312 may be a carbonization stage, wherein an intermediate temperature T1 is sufficient to carbonize the substrate supporting the material to be sintered. For example, the intermediate temperature T1 may be in the range of 200-500°C (inclusive). In some embodiments, the intermediate temperature T1 is a base temperature inside the shell of the sintering furnace but outside the heating zone. Alternatively or additionally, the intermediate temperature T1 may be generated by a separate heating element within the sintering furnace (e.g., a heating element disposed along a travel path between the inlet and the sintering heating zone). Alternatively or additionally, the intermediate temperature T1 may be generated by a separate heating element within the sintering furnace (e.g., a heating element disposed along a travel path between the inlet and the sintering heating zone). I It can be generated by a separate heating element outside the sintering furnace (e.g., a separate heating element upstream of the inlet of the sintering furnace shell, or an external heating element located only before the inlet of the sintering furnace shell).

[0078] In some embodiments, the duration t3 of the preheating stage 312 may be greater than the sintering duration t1 and / or the conveying duration t2. Alternatively, the duration t3 of the preheating stage 312 may be less than either or both of t1 and t2. In some embodiments, for example, when carbonization of the upstream substrate occurs simultaneously with sintering of the material on the downstream substrate, the duration t3 of the preheating stage 312 may be substantially equal to t1. Alternatively, in some embodiments, the duration t3 of the preheating stage 312 may be substantially equal to t2, for example, when carbonization occurs on the substrate en route into the heating zone.

[0079] In some embodiments, after the preheating stage 312, the material can pass through a transfer stage 314 before entering the sintering stage 302. For example, the transfer stage 314 may correspond to the time required for the material to move from the preheating region (e.g., the shell upstream of the sintering furnace, or a region within the furnace but upstream of the sintering heating region) to the sintering heating region. In some embodiments, the duration t4 of the transfer stage 314 may be substantially equal to t2, for example, when the upstream material moves out of the preheating region, the downstream substrate also moves out of the sintering heating region. Alternatively or additionally, the duration t4 of the transfer stage 314 may be zero or close to zero, for example, directly from the intermediate temperature T in the sintering stage 302. I Instead of from the base temperature T L If it has already begun.

[0080] Computer implementation

[0081] Figure 2 A general example of a suitable computing environment 231 is described, in which the described innovations, such as various aspects of controller 122 and / or the operating methods of any disclosed sintering furnace system, can be implemented. The computing environment 231 is not intended to impose any limitations on its scope of use or functionality, as the innovations can be implemented in a variety of general-purpose or specialized computing systems. For example, the computing environment 231 can be any of a variety of computing devices, such as desktop computers, laptops, server computers, tablets, etc.

[0082] The computing environment 231 includes one or more processing units 235, 237 and memory 239, 241. Figure 2 In this configuration, 251 is included within the dashed lines. Processing units 235 and 237 can execute computer-executable instructions. Processing units can be general-purpose central processing units (CPUs), processors in application-specific integrated circuits (ASICs), or any other type of processor. In a multiprocessor system, multiple processing units execute computer-executable instructions to increase processing power. For example, Figure 2 A central processing unit 235 and a graphics processing unit or coprocessor 237 are shown. Tangible memory 239, 241 may be volatile memory (such as registers, cache memory, RAM), non-volatile memory (such as ROM, EEPROM, flash memory, etc.), or some combination thereof, accessible by the processing unit. Memory 239, 241 stores one or more innovative software 233 implementing the invention in the form of computer-executable instructions suitable for execution by the processing unit.

[0083] The computing system may have additional features. For example, computing environment 231 includes memory 261, one or more input devices 271, one or more output devices 281, and one or more communication connections 291. Interconnection mechanisms (not shown), such as buses, controllers, or networks, interconnect the various components of computing environment 231. Typically, operating system software (not shown) provides an operating environment for other software executing in computing environment 231 and coordinates the activities of the various components of computing environment 231.

[0084] The tangible memory 261 may be removable or non-removable and includes a magnetic disk, magnetic tape or cassette tape, CD-ROM, DVD, or any other medium that can be used to store information in a non-transitory manner and can be accessed within the computing environment 231. The memory 261 may store instructions for the software 233 to implement one or more of the innovations described herein.

[0085] Input device 271 may be a touch input device (such as a keyboard, mouse, pen, or trackball), voice input device, scanning device, or other device that provides input to computing environment 231. Output device 271 may be a monitor, printer, speaker, CD burner, or other device that provides output from computing environment 231.

[0086] Communication connection 291 allows communication with another computing entity via a communication medium. The communication medium transmits information, such as computer-executable instructions, audio or video input or output, or other data in modulated data signals. Modulated data signals are signals whose characteristics are set or altered in a manner that encodes information within them. For example, the communication medium may be electrical, optical, radio frequency (RF), or other carriers, but is not limited to these.

[0087] Any of the disclosed methods can be implemented as computer-executable instructions stored on one or more computer-readable storage media (e.g., one or more optical media, optical discs, volatile memory components (such as DRAM or SRAM), or non-volatile memory components (such as flash memory or hard disk drives)) and executed on a computer (e.g., any commercial computer, including smartphones or other mobile devices containing computing hardware). The term "computer-readable storage medium" excludes communication connections such as signals and carrier waves. Any computer-executable instructions used to implement the disclosed techniques, as well as any data created and used during the implementation of the disclosed embodiments, can be stored on one or more computer-readable storage media. For example, the computer-executable instructions can be part of a dedicated software application or part of a software application accessed or downloaded via a web browser or other software application (such as a remote computing application). Such software can, for example, execute on a single local computer (such as any suitable commercial computer) or in a networked environment (e.g., via the Internet, a wide area network, a local area network, a client-server network (such as a cloud computing network), or other such networks) using one or more network computers.

[0088] For clarity, this document describes only selected aspects of software-based implementations. Other details well-known in the art have been omitted. For example, it should be understood that the disclosed techniques are not limited to any particular computer language or program. For instance, aspects of the disclosed techniques can be implemented using software written in C++, Java, Perl, or any other suitable programming language. Similarly, the disclosed techniques are not limited to any particular computer or hardware type. Certain details of suitable computers and hardware are well-known and need not be described in detail in this disclosure.

[0089] It should also be fully understood that any function described herein can be performed, at least in part, by one or more hardware logic components instead of software. Examples of usable hardware logic components include, but are not limited to, field-programmable gate arrays (FPGAs), application-specific integrated circuits (ASICs), application-specific standard products (ASSPs), system-on-a-chip (SoCs), complex programmable logic devices (CPLDs), etc.

[0090] Furthermore, any software-based embodiment (including, for example, computer-executable instructions for causing a computer to perform any of the disclosed methods) can be uploaded, downloaded, or remotely accessed via suitable communication means. These suitable communication means include the Internet, the World Wide Web, intranets, software applications, cable (including fiber optic cables), magnetic communication, electromagnetic communication (including radio frequency, microwave, and infrared communication), electronic communication, or other such communication means. In any of the foregoing examples and embodiments, the provision of requests (such as data requests), indications (such as data signals), instructions (such as control signals), or any other communication between systems, components, devices, etc., can be achieved by generating and transmitting suitable electrical signals via wired or wireless connections.

[0091] Heating element configuration

[0092] In some embodiments, the heating components of the sintering furnace system may include a Joule heating element, a power supply, and wires coupling the Joule heating element to the power supply. For example, Figure 4A A heating assembly 400 with a Joule heating element 402 is shown. A power supply 404 (such as a current source) is electrically connected to opposite ends of the Joule heating element 402 via respective lines 406a, 406b. In some embodiments, the Joule heating element 402 may be composed of a conductive carbon material, such as carbon nanofibers, carbon paper, carbon felt, carbon cloth, graphite paper, graphite felt, graphite cloth, graphite film, and / or graphite plate. Alternatively or additionally, the Joule heating element 402 may be composed of other conductive materials, such as refractive metals (e.g., tungsten). Although Figure 4A A Joule heating element is shown formed as a rectangular sheet or film (e.g., having a width of about 2 cm and a length of about 10 cm), but other shapes (e.g., regular or arbitrary shapes) are also possible depending on one or more of the intended embodiments. In some embodiments, the heating element 402 can be heated from room temperature to the sintering temperature in about 30 seconds or less, followed by a sintering time of about 10 seconds, and then a rapid cooling time of about 5 seconds.

[0093] In some embodiments, the heating assembly may include features that compensate for mechanical changes caused by thermal shock profiles, such as thermal expansion of the heating element due to heating to the sintering temperature and subsequent thermal contraction due to cooling from the sintering temperature. For example... Figures 4B to 4CAn exemplary heating assembly 410 with electrically coupled components 412a, 412 is shown for accommodating changes in the size / shape of the heating element 402 caused by thermal shock profiles. For example, each electrically coupled component 412a, 412b may include a biasing clip 414 having a pair of angled members or arms 422. The electrically coupled components 412a, 412b may also include a pair of conductive plates 416, 418 that cooperate to clamp the end of the heating element 402 within a recess 420 between them. The angled arms 422 of each biasing clip 414 can effectively press the plates 416, 418 together, thereby reliably clamping the end of the heating element 402. For example, the height of the recess 420 may be less than the thickness of the heating element 402, such that the plates 416, 418 partially compress and clamp the end of the heating element 402. In some embodiments, components of the electrical coupling assembly may be conductive, for example, such that the electrical connection from the power supply 404 to the heating element 402 can be achieved by connecting wires 406a, 406b to corresponding bias clips 414. For example, each bias clip 414 may be formed of metal (e.g., copper, copper-plated stainless steel, etc.), and each plate 416, 418 may be formed of a conductive carbon-based material (e.g., graphite). In some embodiments, lines 406a, 406b may be formed of a refractory metal (e.g., tungsten or a combination of copper and silver). The configuration of the coupling assemblies 412a, 412b effectively allows for the expansion / contraction of the heating element while maintaining good electrical contact with the heating element and at least partially insulates the metal lines and / or metal clips from the high temperatures generated by the heating element that would otherwise melt or degrade the constituent metals.

[0094] Two-stage heating configuration

[0095] In some embodiments, multiple heating stages may be provided within the shell of the same furnace, for example, to provide preheating (e.g., for substrate carbonization, for precursor drying, or for any other purpose). For example, Figure 5AA two-stage sintering furnace system 500 is shown, which may have a housing 508 including and / or defining an inlet 502, an outlet 506, and an internal volume 504 disposed between the inlet 502 and the outlet 506 along the direction of travel. In operation, a conveyor belt 522 can be used to transport material 512i to be sintered on a substrate 510i (e.g., a polymer film) via the inlet 502 into the internal volume 504 of the housing 508. The substrate 510i and the precursor material 512i can be positioned by the conveyor belt 522 during a preheating stage 514, for example, within the heating region of a first heating element 516. In some embodiments, the preheating stage 514 can effectively convert the substrate into a carbide material 510c. After the preheating stage 514, the conveyor belt 522 can reposition the carbide material 510c and the precursor material 512i during the sintering stage, for example, within the heating region 124 of the sintering heating element 116. In some embodiments, the sintering stage 524 can effectively convert the precursor material 512i into the sintered material 512s.

[0096] For example, in some embodiments, the first heating element 516 may be a Joule heating element, which is operatively coupled to a power supply 518 (which may be different from or integrated into the power supply 118 driving the sintering heating element 116) via a line passing through a corresponding electrical conductor feedthrough or passage 520a, 520b. Alternatively, in some embodiments, the first heating element 516 may employ another heating mechanism (e.g., capable of producing temperatures below 500°C). In some embodiments, the controller 122 may control the operation of the heating elements 516, 116 during the preheating stage 514 and the sintering stage 524. Alternatively, in some embodiments, a separate controller may be provided for each stage 514, 524, with or without communication between them to coordinate their operation.

[0097] In some embodiments, multiple heating stages can be provided via the shells of furnaces arranged in series, for example, providing initial preheating (e.g., for substrate carbonization, for precursor drying, or for any other purpose), followed by sintering. For example, Figure 5B A two-stage sintering furnace system 500 is shown, which may have a first heating stage 544 (e.g., a preheating stage) and a second heating stage 554 (e.g., a sintering stage). The first heating stage 544 may include a first housing 538, which includes and / or defines a first inlet 532, a first outlet 536, and a first internal volume 534 disposed along the travel direction between the first inlet 532 and the first outlet 536. In some embodiments, the second heating stage 554 may have the same characteristics as the second heating stage. Figure 1A The sintering furnace system 100 or any other sintering furnace system disclosed herein has a similar configuration (e.g., shell 108, sintering heating element 116, etc.).

[0098] In operation, a conveyor belt 542 can be used to transport the material 512i to be sintered on the substrate 510i (e.g., a polymer film) into the first internal volume 534 of the first housing 538 (e.g., via inlet 532 to a location within the heating region of the first heating element 546). In some embodiments, the first heating stage 544 can effectively convert the substrate into a carbide material 510c. After the first heating stage 544, the conveyor belt 542 can transport the carbide material 510c and the precursor material 512i out of the housing 538 via outlet 536 and into the inlet 110 of the housing 108 for the second heating stage 554, for example, to a location within the heating region 124 of the sintering heating element 116. In some embodiments, the sintering stage 554 can effectively convert the precursor material 512i into the sintered material 512s.

[0099] For example, in some embodiments, the first heating element 546 may be a Joule heating element, which is operatively coupled to a power supply 548 (which may be different from or integrated into the power supply 118 driving the sintering heating element 116) via a line passing through a corresponding electrical conductor feedline or passage 550a, 550b. Alternatively, in some embodiments, the first heating element 546 may employ another heating mechanism (e.g., capable of producing temperatures below 500°C). In some embodiments, the controller 122 may control the operation of the heating elements 546, 116 in the first heating stage 544 and the second heating stage 554. Alternatively, in some embodiments, a separate controller may be provided for each stage 544, 554, with or without communication between them to coordinate their operation.

[0100] Multiple heating element configuration

[0101] In some embodiments, multiple heating elements may be arranged within the shell of the same furnace, for example, to process multiple materials to be sintered simultaneously or sequentially in batches. For example, Figure 6 A batch processing sintering furnace system 600 is shown, which may have a housing 616 including and / or defining an inlet 610, an outlet 612, and an internal volume 614 disposed along the direction of travel between the inlet 610 and the outlet. The batch processing sintering furnace system 600 may also include a plurality of heating elements 116 arranged within the internal volume 614, and, for example, arranged such that the respective heating zones 124 are arranged in series along the direction of travel to form a first heating stage 604, a second heating stage 606, and a third heating stage 608. Although in Figure 6 The example shows three heating stages 604 to 608, but fewer or more stages are possible depending on one or more intended embodiments.

[0102] During operation, a batch of material 128i to be sintered can be transported via conveyor belt through inlet 610 into internal volume 614. Figure 6 In the example shown, two materials 128i are placed in each heating zone 124; however, in some embodiments, fewer (e.g., one material 128i) or more (e.g., three or more materials 128i) of materials may be placed in each heating zone 124. In some embodiments, to process batch 602 of material 128i, the heating element 116 may be energized simultaneously to provide thermal shock profiles to the material 128i in the various heating zones 124 of stages 604 to 608, thereby simultaneously forming multiple sintered materials 128s. This batch of sintered materials 128s can then be transported out of the internal volume 614 via an outlet 612 using a conveyor belt, while the next batch of material 128i to be sintered is loaded via an inlet 610. Alternatively or additionally, in some embodiments, heating stages 604 to 608 may operate at different times rather than in parallel. For example, heating element 116 of the first stage 604 provides a thermal shock profile to the material in its heating region, followed by heating element 116 of the second stage 606 providing a thermal shock profile to the material in its heating region, and so on. Once all material in the batch has been sintered, the conveyor belt can remove the batch of material from the housing 616 and / or load the next batch of material into the housing for processing.

[0103] Cooling system configuration

[0104] Because the thermal shock profile generates high temperatures (e.g., 1000-3000°C) within the shell of the sintering furnace, the outer surface of the shell may exhibit temperatures harmful to the surrounding environment and / or the operator (e.g., 100°C or higher). Alternatively or additionally, the high temperatures of the thermal shock may compromise the integrity of the sintering furnace, for example, by subjecting the shell walls to temperatures approaching or exceeding the melting temperature of its constituent materials. Therefore, in some embodiments, a cooling system may be provided to maintain the temperature of the sintering furnace walls and / or the temperature of the outer surface of the shell at or below a predetermined temperature.

[0105] For example, Figure 7A A sintering furnace system 700 is shown, which employs a cooling system in thermal communication with the outer surface of a housing 108. In the illustrated example, the cooling system may include a first fluid conduit 704 disposed near, above, or within the top surface 706 of the housing 108, and a second fluid conduit 714 disposed near, above, or within the bottom surface 716 of the housing 108. In some embodiments, additional conduits in thermal communication with other surfaces of the housing 108 (e.g., similar to...) may also be provided. Figures 15A to 15C(Configuration of the fluid conduits). Alternatively or additionally, in some embodiments, fluid conduits may be disposed on fewer surfaces of the housing 108 or on a portion of the housing. In some embodiments, each fluid conduit 704, 714 may have a meandering or tortuous configuration, such that fluid flow therethrough may be in a direction orthogonal to or at least intersecting with the direction of travel T of the material within the housing 108. In some embodiments, the fluid flowing through the conduits 704, 714 may include any type of heat transfer fluid, such as, but not limited to, water, oil, molten salt, etc.

[0106] In some embodiments, fluid may flow serially through conduits 704 and 714. For example, a hydraulic pump 708 may be used to guide fluid from the outlet of the first conduit 704 through inlet line 720 to the second conduit 714, and from the outlet of the second conduit 714 through outlet line 722 to the inlet of the first conduit 704. Alternatively, in some embodiments, fluid may flow in parallel through conduits 704 and 714. For example, the output of the hydraulic pump 708 may simultaneously be directed to the respective inlets of conduits 704 and 714, while the discharge from the outlets of conduits 704 and 714 may be redirected to the input of the hydraulic pump 708. In both serial and parallel configurations, the direction of fluid flow through the first conduit 704 may be the same as the direction of fluid flow through the second conduit 714. Alternatively, the direction of fluid flow through the first conduit 704 may be opposite to the direction of flow through the second conduit 714.

[0107] In some embodiments, controller 122 may control the cooling system to control its operation, thereby maintaining the external temperature of housing 108 below a predetermined threshold (e.g., below 100°C, or below 50°C, or below 30°C), for example, based on sensors (e.g., thermocouples, not shown) mounted on the external surface and / or according to thermal imaging of the external surface of the furnace housing. In some embodiments, controller 122 may be operably coupled to hydraulic pump 708, for example, to control the fluid velocity through conduits 704, 714. In some embodiments, the output of one or more conduits may be directed to heat exchanger 710 (e.g., crossflow heat exchanger) to cool the fluid in conduits 704, 714, for example, by exchanging heat with cooling fluid flow 718 (e.g., air, water, oil, etc.). In some embodiments, in addition to heat exchanger 710, or instead of heat exchanger 710, heat dissipation devices (e.g., needle-finned radiators, straight-finned radiators, or diffuser-finned radiators) may be used to cool the fluid in conduits 704 and 714.

[0108] exist Figure 7A In the examples shown, catheters 704 and 714 have a meandering construction; however, other catheter constructions are possible according to one or more of the intended embodiments. For example, Figure 7BA sintering furnace system 730 employing a cooling system is shown, in which first and second fluid conduits 734, 744 are respectively disposed near, above, or within surfaces 706, 716. Each fluid conduit 734, 744 may have a substantially straight configuration, for example, extending parallel to the direction of material travel T within the furnace shell 108. In some embodiments, a hydraulic pump 708 is used, for example, to simultaneously direct fluid to its inlet via an inlet line 750, thereby allowing fluid to flow parallel through conduits 734, 744, and to reintroduce fluid discharged from conduits 734, 744 into the input of pump 708 via an outlet line 752. Alternatively, in some embodiments, the fluid may be in a similar manner... Figure 7A The flow is sequential through conduits 734 and 744 as shown.

[0109] Protective gas configuration

[0110] In some embodiments, a directional inert gas flow may be provided to the internal volume of the sintering furnace, for example, to increase the cooling rate at the end of the thermal shock curve, extend the lifespan and / or improve the reliability of the heating elements, prevent contaminants from entering the heating zone, the material to be sintered and / or the sintered material, and / or for any other purpose. For example, Figures 8A to 8B A heating assembly 800 is shown, which is formed by a pair of heating elements 802a, 802b on opposite sides of a material 810 to be sintered. Electrical wires 804 (e.g., formed of a refractory metal such as tungsten) may extend from opposite sides of each heating element 802a, 802b (e.g., perpendicular to the direction of travel of the material 810). A first pair of protective gas nozzles 806a, 806b may be disposed on opposite sides of the first heating element 802a (e.g., relative to the direction of travel of the material). A second pair of protective gas nozzles 808a, 808b may be disposed on opposite sides of the second heating element 802b (e.g., relative to a direction orthogonal to the direction of travel of the material). In some embodiments, the protective gas nozzles 806a, 806b, 808a, 808b may be formed of a refractory material (e.g., tungsten or carbide).

[0111] The second pair of protective gas nozzles 808a, 808b may have a different arrangement than the first pair of protective gas nozzles 806a, 806b, for example, to accommodate a conveyor belt extending between the heating elements 802a, 802b and / or to feed and discharge material into and out of the heating area between the heating elements 802a, 802b. In some embodiments, the protective gas nozzles 806a, 806b, 808a, 808b may direct an inert gas flow toward the side ends of the respective heating elements 802a, 802b and / or the back surfaces of the respective heating elements 802a, 802b (e.g., opposite to and / or in contact with the side facing the material 810 to be sintered). Alternatively or additionally, in some embodiments, the inert gas flow may be directed toward the heating area of ​​the heater. For example, Figure 8C An exemplary sintering furnace system 820 is shown, having a furnace housing 822 including and / or defining an inlet 830, an outlet 832, and a pair of protective gas nozzles 824a, 824b. The protective gas nozzles 824a and 824b may be integrally formed with the housing 822 and arranged such that an inert gas flow 826 is directed to a heating zone 124 and exits the internal volume of the housing 822 via the inlet 830 or outlet 832, respectively. Other configurations of the protective gas nozzles and the inert gas flow are also possible according to one or more contemplated embodiments.

[0112] Stress application configuration

[0113] In some embodiments, the thermal shock profile can be applied simultaneously with the application of pressure, for example, via the heating element itself or via another component (e.g., formed of refractory material) within the furnace casing near or adjacent to the heating element. For example, Figure 9 Operation of an exemplary sintering furnace system with pressing is illustrated. In the initial transfer phase 900, the material 128i to be sintered is moved via conveyor belt 126 through inlet 110 to the heating zone 124 within the housing 108. Heating elements 116 may be mounted on a movable platform or actuating member 904 (e.g., a screw mechanism) extending through channel 906 and movable by an actuating assembly 902 (e.g., a rotary motor) controlled by controller 122. In the illustrated example, the actuating assembly 902 may be located outside the housing 108, and the actuating member 904 may extend through channel 906; while in some embodiments, both the actuating member 904 and / or the actuating assembly 902 may be located inside the housing 108. Furthermore, although... Figure 9 A specific type of actuating member and actuating assembly is shown, but other mechanisms may also be used to move the heating element toward or away from the material 128i to be sintered, depending on one or more of the intended embodiments.

[0114] After the transfer phase 900, the operation proceeds to the contact phase 910, in which the actuation assembly 902 moves the heating element 116 toward the material 128i to be sintered in the heating region 124. The operation can then proceed to the sintering phase 920, in which the heating element 116 is energized, causing the material 128i to be subjected to the effects of a thermal shock profile (e.g., as shown in the image). Figure 3A (As shown), after this, the heating element 116 is retracted by the actuation assembly 902 in the release phase 930. Then, the operation can return to the transfer phase 900 to repeat for the next set of materials to be sintered.

[0115] In some embodiments, the heating element 116 may be positioned in the contact phase 910 to reduce the gap between the heating element 116 and the material 128i compared to the transfer phase 900, for example, to provide radiant heating during thermal shock profiling. Alternatively, in some embodiments, the heating element 116 may be positioned in the contact phase 910 to eliminate the gap between the heating element 116 and the material 128i compared to the transfer phase 900, for example, to provide conductive heating during thermal shock profiling. Alternatively or additionally, in some embodiments, the heating element 116 may be positioned in the contact phase 910 to compress the material 128i. In some embodiments, the conveyor belt 126 may be replaced by another heating element, which may be fixed or movable separately toward the heating element 116. Alternatively or additionally, in some embodiments, the conveyor belt 126 may be replaced by a high-temperature platform or support (e.g., formed of a carbon-based or refractory material), or a portion of the conveyor belt 126 may be supported by a high-temperature platform or support, which may be fixed or movable individually toward the heating element 116.

[0116] Integrated heating and transmission configuration

[0117] In some embodiments, the heating element may be integrated with the transmission component or may be part of the transmission component. For example... Figure 10An exemplary sintering furnace system 1000 is illustrated, which employs a portion 1016 of a conveyor belt 1002 as a heating element to subject material 128i within a heating zone 1024 to a desired thermal shock profile. In some embodiments, the portion 1016 may serve as a Joule heating element. In such embodiments, the conveyor belt may be formed of a conductive material, such as carbon, graphite, metal, or combinations thereof. Electrical interfaces 1004a, 1004b may make electrical contact with the portion 1016 and are configured to apply current pulses to the portion 1016 to achieve Joule heating. For example, electrical interfaces 1004a, 1004b may include one or more conductive rollers, one or more slip ring interfaces, etc. In operation, the conveyor belt 1002 may extend between the inlet 1010 and outlet 1012 of the housing 1008 and may be supported within the housing 1008 by support rollers 1006a, 1006b (e.g., arranged within the internal volume 1014 and formed of refractory metal, as shown, or arranged outside the housing and formed of metal). In some embodiments, the housing may further include insulating material 1018, 1022 on opposite sides of the conveyor belt 1002 within the internal volume 1014, for example, to protect the walls of the furnace housing 1008 from excessively high temperatures (e.g., when the size of the housing 1008 is less than 100 times the volume of the heating zone).

[0118] The material 128i to be sintered can be conveyed to the heating zone 1024, where current is applied through the portion 1016 between electrical interfaces 1004a and 1004b, thereby placing the material 128i in the desired thermal shock profile. In some embodiments, the current can be applied while the conveyor belt is stationary, for example, after the material 128i has moved into the heating zone. Alternatively or additionally, in some embodiments, the current can be applied while the conveyor belt continues to move, for example, in a continuous manner. In such embodiments, the speed of the conveyor belt, the size of the heating zone 1024, and / or the timing of the current can be combined and adjusted so that each type of material passing through the heating zone 1024 is in the corresponding thermal shock profile.

[0119] Exemplary sintering furnace system

[0120] Figures 11A to 11BA high-temperature sintering furnace system 1100 and its operation are illustrated, for example, for roll-to-roll processing. The high-temperature sintering furnace system 1100 employs a pair of opposing heating elements (e.g., an upper heating element 1112 for providing radiant heating to the material to be sintered and a lower heating element 1114 for providing conductive heating to the material to be sintered), the material to be sintered being carried by a conveyor belt membrane 1102 (e.g., formed of carbon), which is supported by rollers 1104 (e.g., formed of a metal such as stainless steel). For example, the conveyor belt membrane 1102 can transport a substrate 1128i (e.g., a green belt) having a precursor from an inlet region 1124 to a heating region 1110, as shown in input stage 1100a. In transfer stage 1100b, the substrate 1128i can be transferred from the conveyor belt membrane 1102 by material transfer rollers 1106 (e.g., formed of a refractory metal, such as tungsten) and placed on the upper surface of the heating element 1114 in stage 1100c. Heating elements 1112 and 1114 (e.g., Joule-heated carbon ribbons) can rapidly heat the substrate 128i within the heating zone 1110 to achieve rapid synthesis (e.g., solid-state reaction) and reaction sintering. For example, in an inert atmosphere, heating elements 1112 and 1114 can provide temperatures of at least 2000°C (e.g., ≥3000°C), which is sufficient for synthesizing and sintering ceramic materials. In some embodiments, heating elements 1112 and 1114 can rise from room temperature to the sintering temperature in about 30 seconds or less, then undergo a sintering time of about 10 seconds, and then rapidly cool to room temperature in about 5 seconds. After sintering, the sintered material 1128s can be transferred via a tilting mechanism 1120 (e.g., made of refractory ceramics such as hard alloys), which allows the heating element 1114 to pivot about a rotation axis 1118, as shown in stage 1100d. In the output stage 1100e, the sintered material 1128s can then be moved to the outlet area 1126 via conveyor belt membrane 1102 for further processing or use.

[0121] In some embodiments, any one or both of the heating elements 1112 and 1114 may be composed of a conductive carbon material, such as carbon paper, carbon felt, carbon cloth, graphite paper, graphite felt, graphite cloth, graphite film, or graphite plate. Alternatively or additionally, in some embodiments, other conductive materials or composite materials may be used for the heating elements 1112 and 1114. In some embodiments, the dimensions of the heating elements 1112 and 1114 may be adjusted based on the dimensions of the material 1128i to be sintered and / or manufacturing requirements (e.g., to provide a sufficient yield of material 1128s for sintering). For example, the heating elements 1112 and 1114 may have a width of approximately 2 cm and a length of approximately 10 cm (e.g., in a plane parallel to the material travel direction). Other shapes and dimensions of the heating elements are also possible according to one or more contemplated embodiments. In some embodiments, the distance between the upper heating element 1112 and the material 1128i may be adjusted by a displacement guide 1122, which may be configured to support and / or move the upper heating element. For example, the displacement guide 1122 can be formed of refractory ceramics, such as silicon carbide, boron carbide, etc.

[0122] When heating elements 1112 and 1114 are made of conductive material, they can be heated by a power source (not shown) that supplies current through the conductive material of the heating elements via a line cable 1116 (e.g., formed of a refractory metal such as tungsten or a combination of copper and silver). The amount of current flowing through the conductive material of heating elements 1112 and 1114 corresponds to the heating rate. A controller (not shown) can control the heating rate and the power source by supplying the required current to the conductive material of heating elements 1112 and 1114.

[0123] Figures 12A to 12B Another configuration of the high-temperature sintering furnace system 1200 is shown, for example, for roll-to-roll processing. The operation of the heating elements 1112, 1114, the transfer assembly, and the furnace system 120 can be similar to that described above. Figures 12A to 12BThe description is similar; however, the furnace system 1200 may also include a mechanism for applying pressure to the heating elements 1112, 1114, thereby applying pressure to the material 1128i to be sintered. For example, the pressure applicator 1202 (e.g., a platform) may be controlled via an actuation mechanism 1204 (e.g., a linkage) to apply pressure to the material during sintering, thereby resulting in a higher density of the sintered material. In some embodiments, the applied pressure may be electronically controlled by a controller (not shown) according to the desired density and / or any other parameters. For example, the pressure applicator 1202, the actuation mechanism 1204, or both may be formed of refractory ceramics such as silicon carbide. Optionally, in some embodiments, pressure may be applied to the heating elements 1112, 1114 and the material 1128i by other types of mechanisms (e.g., hydraulic plates, robotic arms / mechanical arms, or any other mechanical pressure application mechanism).

[0124] Figures 13A to 13B Another configuration of the high-temperature sintering furnace system 1300 is shown, for example, for roll-to-roll processing. In the example shown, the upper heating element 1314 is movable and can come into contact with the material 1328i to be sintered via a line conductor guide 1316 (e.g., formed of a refractory material such as tungsten) (e.g., by eliminating the gap 1312 between the heating element 1314 and the conveyor belt membrane 1302). The conveyor belt membrane 1302 (e.g., formed of carbon) can convey materials (e.g., the material 1328i to be sintered and the sintered material 1328s) from the inlet region 1324 to the outlet region 1326 without requiring material to be conveyed to a separate heating element. Conversely, the line current conductor 1306 (e.g., formed of a refractory material such as tungsten) energizes a portion 1308 of the conveyor belt membrane 1302 within the heating zone 1310 to use said portion 1308 as a lower heating element, while the roller 1304 (e.g., formed of a metal such as stainless steel) supports and moves the conveyor belt membrane away from the heating zone 1310. Although not shown in the figures, the transport system for moving the conveyor belt membrane 1302 may include one or more motors, one or more controllers, and / or other conventional components. In some embodiments, the controller may control a power source (e.g., a current source) to heat the heating elements 1308, 1314, and / or control the transport system to advance / leave material into / out of the heating zone 1310, and / or control the conductor guide 1316 to move / leave the upper heating element 1314 into / out of the heating zone 1310.

[0125] Figures 14A to 14B Another configuration of the high-temperature sintering furnace system 1400 is shown, for example, for roll-to-roll processing. The operation of the heating elements 1308, 1314, the transfer assembly, and the furnace system 1400 can be similar to that described above. Figures 13A to 13BThe description is similar; however, the furnace system 1300 may further include a mechanism for applying pressure to the heating elements 1308, 1314, for example, a pressure applicator 1202 (e.g., a pressure plate) controlled via an actuation mechanism 1204 (e.g., a linkage), which operates in the same manner as described above. Figures 12A to 12B The described operation methods are similar.

[0126] Figures 15A to 15C Another configuration of the high-temperature sintering furnace system 1500 is shown, for example, for roll-to-roll processing. The heating elements, transport components, and operation of the furnace system 1500 can be similar to those described above. Figures 12A to 12B The described system 1200 includes heating elements, transport components, and operation; however, the furnace system 1500 may further include a furnace housing 1502 and a cooling system. The furnace housing 1502 may include and / or define one or more protective gas inlets 1506, inlets 1504, and outlets 1514. In some embodiments, a periodically or continuously flowing inert gas stream (e.g., argon, nitrogen, or an argon / hydrogen mixture) may be provided through the gas inlets 1506, for example, to increase the lifespan of the heating elements and / or to provide an inert gas environment within the housing 1502. In some embodiments, the cooling system may include meandering cooling conduits 1508a-1508d disposed on the top, bottom, and side surfaces of the furnace housing 1502 (e.g., in contact with or adjacent to it). Alternatively, in some embodiments, the conduits 1508a-1508d may be integrated into the housing 1502, for example, disposed below the outer surface of the housing 1502 but outside the internal volume of the housing (e.g., embedded within the wall of the housing). Depending on the heating power generated by the heating element, the working fluid flowing through conduits 1508a-1508 can be water, oil, liquid nitrogen, etc. In some embodiments, in order to achieve an ultrafast cooling rate (e.g., at least 100-500°C / s), the dimensional ratio between the heater and the furnace shell (the length of the heating zone to the length of the internal volume (e.g., from the inlet to the outlet)) can be in the range of 100-1000 (inclusive).

[0127] Figures 16A to 16C Another configuration of the high-temperature sintering furnace system 1600 is shown, for example, for roll-to-roll processing. The heating elements, transport components, and operation of the furnace system 1600 can be similar to those described above. Figures 11A to 11BThe described system 1100 includes heating elements, transport components, and operation; however, the furnace system 1600 may further include a furnace housing 1602 having insulating materials 1604, 1606. The furnace housing 1602 may include and / or define one or more protective gas flow channels 1608a, 1608b (e.g., formed in the insulating material 1604), an inlet 1610, and an outlet 1612. In some embodiments, a periodic or continuous flow of inert gas (e.g., argon, nitrogen, argon / hydrogen mixture) may be provided via the gas flow channels 1608a, 1608b (e.g., via gas inlet 1614) for example, to increase the lifespan of the heating element and / or to provide an inert gas environment within the housing 1602. For example, the insulating materials 1604, 1606 may be formed of glass fiber, porous ceramics, aerogel, etc. In some embodiments, the dimensions (e.g., thickness) of the insulation materials 1604, 1606 may be determined based on the maximum temperature required for the exterior or outer surface of the furnace shell 1602 during the thermal shock process and based on the corresponding thermal conductivity of the insulation materials.

[0128] To illustrate the relative dimensions between furnace systems with and without insulation materials Figure 17A The above is shown Figures 15A to 15B A similar sintering furnace system 1500, Figure 17B The above is shown Figures 16A to 16B A similar sintering furnace system 1600. In some embodiments, the use of insulating materials allows furnace system 1600 to be much smaller than furnace system 1500 in terms of both external footprint and internal volume (e.g., volume 1620 is much larger than volume 1510). To achieve adequate cooling (with or without active cooling) in the larger furnace system 1500, the size of internal volume 1510 can be much larger than the volume of heating zone 1512. The positioning and / or size of the heating zone relative to the sidewalls of internal volume 1510 can also be customized to allow adequate cooling at the end of the thermal shock profile and / or minimize or reduce the transfer of high temperatures to the outside of the shell.

[0129] For example, L 入口 (e.g., the length from the inlet 1504 to the nearest end of the heating region 1512 (e.g., the edge of the heating element 1114), L) 出口 (e.g., the length from outlet 1514 to the nearest end of heating zone 1512 (e.g., the edge of heating element 1114)) or both may be greater than (e.g., at least 5 times or at least 50 times) the width of heating zone 1512. Alternatively or additionally, L 顶部 (For example, the height from the top of the internal volume 1510 to the nearest end of the heating region 1512 (e.g., the top surface of the heating element 1114), L) 底部(For example, the height between the bottom of the internal volume 1510 and the nearest end of the heating region 1512 (e.g., the top surface of the heating element 1114)) or both may be greater than (e.g., at least 5 times or at least 50 times) the height of the heating region.

[0130] Figures 18A to 18B Another configuration of the high-temperature sintering furnace system 1800 is shown, for example, for roll-to-roll processing. The high-temperature sintering furnace system 1800 employs a pair of opposing heating elements, such as an upper heating element 1808 and a lower heating element 1818, for heating material carried between a conveyor plate 1810. In the illustrated roll-to-roll configuration, the conveyor plate 1810 can be supplied from an input roller 1820, via a conveyor roller 1824 (e.g., formed of a refractory metal such as tungsten) to the heating region between the heating elements 1808 and 1818, and then wound onto an output roller 1822 after sintering. The sintering furnace system 1800 may also have a pair of main housing members 1802, 1812 disposed on opposite sides of the heating region, with the heating elements 1808, 1818 disposed between the main housing members 1802, 1812. The sintering furnace system 1800 may also provide a first pair of auxiliary shell members 1804a on opposite sides of the transfer substrate 1810 at the inlet end of the heating zone, and a second pair of auxiliary shell members 1804b on opposite sides of the transfer substrate 1810 at the outlet end of the heating zone. The first pair of auxiliary shell members 1804a may cooperate to form an inlet through which the transfer substrate 1810 extends, and the second pair of auxiliary shell members 1804b may cooperate to form an outlet through which the transfer substrate 1810 extends. In some embodiments, the main shell member 1802 may cooperate with adjacent auxiliary shell members 1804a, 1804b to form corresponding inlet conduits 1806a, 1806b for the flow of inert gas, and the main shell member 1812 may cooperate with adjacent auxiliary shell members 1804a, 1804b to form corresponding inlet conduits 1816a, 1816b for the flow of inert gas.

[0131] Figure 19AAnother configuration of the high-temperature sintering furnace system 1900 is shown, for example, employing a continuous conveyor belt setup. The conveyor belt membrane 1908 can carry material 1912i to be sintered (e.g., a precursor substrate, such as a green belt), which is loaded by a sample feed mechanism 1910 (e.g., a machine placement unit) into an input area 1914 upstream of the heating zone 1916. The conveyor belt membrane 1908 can be moved by one or more drive rollers 1902, 1906 and supported by one or more redirection rollers 1904, for example, to position the material 1912i within the heating zone 1916 of the heating elements 1918, 1924. The heating elements 1918, 1924 can be moved toward the material 1912i (e.g., with a spacing of 5-20 cm between heating elements) and / or come into contact with the material 1912i, for example, via a shift guide 1920 (e.g., formed of refractory ceramics such as carbides). For example, by applying current to heating elements 1918 and 1924 via lines 1922 and 1926 (e.g., formed of refractory metals such as tungsten), material 1912i can be rapidly heated by radiation and / or conduction to create a uniform high-temperature environment that transforms the material 1912i to be sintered into the sintered material 1912s. For example, in the outlet area 1930 downstream of heating zone 1916, the sintered material 1912s can be removed from the conveyor belt membrane 1908 using a sample selection mechanism 1928 (such as a machine pick-up unit). Although a single heating zone 1916 is used to process a single material 1912i at a time, multiple heating elements 1918a-c, 1924a-c and corresponding heating zones can also be provided for the simultaneous batch processing 1956 of multiple materials 1912i, for example... Figure 19B The system is shown in 1950.

[0132] Figure 20Another configuration of the high-temperature sintering furnace system 2000 is shown, for example, employing a continuous conveyor belt setup. The conveyor belt membrane 2008 can carry material 2014i to be sintered (e.g., material precursor particles, such as powder), which is deposited from the particle distributor 2012 into the input region 2018 upstream of the heating region 2016. The conveyor belt membrane 2008 can be moved by one or more drive rollers 2002, 2006 and supported by one or more redirection rollers 2004, for example, to position the material 2014i within the heating region 2016 of the heating elements 1918, 1924. The heating elements 1918, 1924 can be moved toward the material 2014i (e.g., with a spacing of 5-20 cm between heating elements) and / or come into contact with the material 2014i, for example, via a displacement guide 1920 (e.g., formed of refractory ceramics such as carbides). For example, by applying current to heating elements 1918 and 1924 via lines 1922 and 1926 (e.g., formed of refractory metals such as tungsten), material 2014i can be rapidly heated via radiation and / or conduction to create a uniform high-temperature environment that transforms the material 2014i to be sintered into sintered material 2014s (e.g., sintered particles). For example, in the outlet zone 2020 downstream of the heating zone 2018, the sintered material 2014s can be removed from the conveyor membrane 2008 and collected in the particle collector 2022. Alternatively or additionally, in some embodiments, the precursor material can be integrated with the conveyor membrane 2008 (e.g., pre-deposited on or embedded in the conveyor membrane 2008) (e.g., in a roll-to-roll arrangement), in which case the particle distributor 2012 and / or collector 2022 can be omitted.

[0133] Figures 21A to 21B Another configuration of the high-temperature sintering furnace system 2100 is shown, for example, employing a fly-through porous reactor setup. System 2100 may have a porous heating element 2118, which is electrically connected to a power source, for example, via electrical contacts 2122a, 2122b (e.g., conductive paste, such as silver paste). Although Figure 21AA single heating element 2118 is shown, but in some embodiments, multiple heating elements may be provided, for example, in a series arrangement (e.g., the spacing between consecutively arranged heaters is 1-5 cm (inclusive)). One or more precursor powders 2114i (e.g., metal nitrites, metal chlorides, etc.) may be provided via a particle distributor 2112 to a fluid suspension mixing manifold 2106 (e.g., a powder injection zone), in which the precursor powders 2114i are combined with a carrier gas 2104 (e.g., an inert gas such as argon, nitrogen, etc.) and carried by the carrier gas 2104 to a gas inlet 2102. The gas-powder flow is sequentially provided to an inlet interface 2108 to enter the furnace's internal volume 2110 (e.g., a quartz tube). The airflow carries particles 2114i to the heating zone 2116 and through the porous heating element 2118 (e.g., with a pore size ranging from 10 μm to 10 mm (inclusive)), thereby subjecting the particles to a thermal shock profile to transform them into sintered particles 2114s. The sintered particles 2114s can exit the furnace at the outlet interface 2120 and can be separated from the outlet airflow 2124 by a sampler 2122 (e.g., a filter element or mesh with a sufficiently small size to capture the particles 2114s).

[0134] Figure 22 Another configuration of the high-temperature sintering furnace system 2200 is shown, for example, using a gravity-dependent fly-through reactor setup. Similar to system 2100, one or more precursor particles 2214i (e.g., metal nitrites, metal chlorides, etc.) can be supplied via particle distributor 2212. These particles flow under the influence of gravity 2206 from the inlet end 2202 to the outlet end 2208 of the heating zone between a pair of heating elements 2204a, 2204b (e.g., arranged substantially parallel to the direction of gravity). As the particles 2214i pass between the heating elements 2204a, 2204b, they undergo thermal shock, transforming into sintered particles 2214s, which are then collected by particle collector 2210.

[0135] Other examples of the disclosed technology

[0136] In view of the embodiments of the subject matter disclosed above, this application discloses additional examples of the clauses listed below. It should be noted that a feature of a single clause, or a combination of more than one feature of the clause, and optionally, a combination with one or more features of one or more other clauses, are also further examples falling within the scope of this application.

[0137] Clause 1. A sintering furnace, comprising:

[0138] A shell that defines the internal volume, the inlet of the internal volume, and the outlet of the internal volume;

[0139] At least one heating element is disposed within the internal volume of the housing and located between the inlet and the outlet, and each heating element is configured to cause the heating zone to be within a temperature profile.

[0140] A transfer assembly for moving one or more substrates into, within, and out of a housing; and

[0141] A control system operably coupled to at least one heating element and a conveying assembly, the control system including one or more processors and a computer-readable storage medium storing instructions, which, when executed by the one or more processors, enable the control system to:

[0142] (a) A first substrate having one or more precursors is moved through an inlet to a heating zone via a transfer assembly;

[0143] (b) By means of at least one heating element, the first substrate in the heating zone is brought to a first temperature of at least 500°C for a first time period; and

[0144] (c) The first substrate having one or more sintered materials on it is removed from the heating zone via an outlet through a conveying assembly.

[0145] Clause 2. A sintering furnace according to any clause or example herein, particularly the sintering furnace of Clause 1, wherein at least one heating element comprises a Joule heating element formed of carbon, graphite, metal or any combination of the above materials.

[0146] Clause 3. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 1 to 2, wherein at least one heating element is formed as a sheet or film.

[0147] Clause 4. For each heating element, the sintering furnace pursuant to any clause or example herein, particularly any sintering furnace pursuant to clauses 1 to 3, further includes:

[0148] A first conductive clamp is coupled to the first end of a corresponding heating element;

[0149] A second conductive clamp is coupled to the second end of a corresponding heating element, the position of which is opposite to the position of the first end;

[0150] A first metal clamp, coupled to the first conductive clamp, applies a clamping force to the first conductive clamp and the first end of the corresponding heating element; and

[0151] A second metal clamp is coupled to the second conductive clamp and applies a clamping force to the second conductive clamp and the second end of the corresponding heating element.

[0152] Clause 5. Sintering furnaces according to any clause or example herein, particularly sintering furnaces according to Clause 4, wherein:

[0153] The first conductive clamp, the second conductive clamp, or both may include one or more graphite plates;

[0154] The first metal clip, the second metal clip, or both include a copper clip or a stainless steel clip with a copper coating; or

[0155] Any combination of the above.

[0156] Clause 6. Sintering furnaces pursuant to any clause or example herein, particularly sintering furnaces pursuant to any of Clauses 4 to 5, also include:

[0157] Current source; and

[0158] The wire couples the current source to the first metal clip and the second metal clip.

[0159] The control system is operatively coupled to the current source, and the computer-readable storage medium stores instructions that cause the control system to control the current source, which, when executed by one or more processors, cause the current source to apply current pulses to at least one heating element via wires, thereby placing the first substrate at a first temperature.

[0160] Clause 7. Sintering furnaces according to any clause or example herein, particularly sintering furnaces according to Clause 6, wherein the wires comprise refractory metals or are formed of tungsten.

[0161] Clause 8. Sintering furnaces according to any clause or example herein, particularly sintering furnaces according to any of clauses 1 to 7, wherein:

[0162] The ratio of the travel length between the inlet and outlet within the casing to the length of the heating zone is at least 100:1;

[0163] The ratio of the internal volume to the volume of the heating zone is at least 100:1; or

[0164] Both of the above.

[0165] Clause 9. Sintering furnaces according to any clause or example herein, particularly sintering furnaces according to clauses 1 to 7, wherein:

[0166] The ratio of the travel length to the length of the heating area ranges from 100:1 to 1000:1, including 100:1 and 1000:1;

[0167] The ratio of the internal volume to the volume of the heating zone ranges from 100:1 to 1000:1, including 100:1 and 1000:1; or

[0168] Both of the above.

[0169] Clause 10. Sintering furnaces according to any clause or example herein, particularly sintering furnaces according to any of clauses 1 to 9, wherein:

[0170] The first temperature range is 1000 to 3000℃ (inclusive);

[0171] The duration of the first time period is less than or equal to 60 seconds;

[0172] The duration of the first time interval is approximately 10 seconds;

[0173] At the start of the first time period, the heating slope to reach the first temperature is at least 10. 2 ℃ / s;

[0174] At the end of the first time period, the cooling slope from the first temperature is at least 10. 3 ℃ / s, or;

[0175] Any combination of the above.

[0176] Clause 11. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 1 to 10, wherein:

[0177] The first substrate comprises a polymer; and

[0178] A computer-readable storage medium stores additional instructions that, when executed by one or more processors, cause the control system to proceed prior to step (b):

[0179] (d) Carbonizing the polymer of the first substrate by bringing the first substrate to a temperature below a first temperature via at least one heating element or another heating element within the housing.

[0180] Clause 12. Sintering furnaces according to any clause or example herein, particularly sintering furnaces according to any of clauses 1 to 10, wherein:

[0181] The first substrate comprises a polymer; and

[0182] A computer-readable storage medium stores additional instructions that, when executed by one or more processors, cause the control system to proceed prior to step (a):

[0183] (d) Carbonizing the polymer of the first substrate by subjecting the first substrate to a temperature lower than a first temperature via at least one external heating element.

[0184] Clause 13. A sintering furnace according to any clause or example of this document, particularly a sintering furnace according to any of clauses 11 to 12, wherein the temperature in step (d) is below 200°C.

[0185] Clause 14. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 11 to 13, wherein the duration of the time period of step (d) is greater than the duration of the first time period of step (b).

[0186] Clause 15. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 1 to 14, wherein the conveying assembly comprises one or more support rollers, one or more conveying rollers, one or more rotary actuators, a conveyor belt, or any combination of the foregoing components.

[0187] Clause 16. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 1 to 15, wherein the conveying components include:

[0188] One or more first conveyor rollers are disposed prior to the heating zone and configured to separate the first substrate from the conveyor belt and convey the first substrate to the heating zone; and

[0189] One or more second transfer rollers are disposed after the heating zone and configured to transfer the first substrate from the heating zone to the conveyor belt.

[0190] Clause 17. A sintering furnace according to any clause or example of this document, particularly a sintering furnace according to any of clauses 15 to 16, wherein the conveyor belt passes around or below the heating zone.

[0191] Clause 18. Sintering furnaces according to any clause or example herein, particularly sintering furnaces according to any of clauses 15 to 17, wherein:

[0192] One or more support rollers comprise one or more metals;

[0193] One or more support rollers are made of stainless steel;

[0194] One or more conveyor rollers comprise one or more refractory metals;

[0195] One or more conveyor rollers are made of tungsten;

[0196] The conveyor belt is made of carbon; or

[0197] Any combination of the above.

[0198] Clause 19. Sintering furnaces according to any clause or example herein, particularly sintering furnaces according to any of clauses 15 to 18, wherein:

[0199] At least one heating element includes a first heating element disposed in a heating region to support a first substrate, the first heating element being configured to heat the first substrate via conduction.

[0200] Clause 20. A sintering furnace according to any clause or example herein, particularly the sintering furnace of Clause 19, further includes a transfer actuator configured to move a first heating element between a first position and a second position, the first position supporting a first substrate in a substantially horizontal direction, and the second position being angled relative to the horizontal direction such that the first substrate slides from the heating region.

[0201] Clause 21. A sintering furnace according to any clause or example of this document, particularly the sintering furnace of Clause 20, wherein the conveying actuator comprises refractory ceramic or is formed of carbide.

[0202] Clause 22. A sintering furnace pursuant to any clause or example herein, particularly a sintering furnace pursuant to any of clauses 15 to 21, wherein:

[0203] At least one heating element includes a second heating element spaced apart from the first substrate in the heating region;

[0204] The second heating element can be actuated between a third position away from the first substrate and a fourth position in contact with the first substrate; and

[0205] The second heating element is configured to heat the first substrate via conduction.

[0206] Clause 23. A sintering furnace pursuant to any clause or example herein, particularly a sintering furnace pursuant to any of clauses 15 to 21, wherein:

[0207] At least one heating element includes a second heating element spaced apart from the first substrate in the heating region;

[0208] The second heating element can be actuated between a third position away from the first substrate and a fourth position close to the first substrate; and

[0209] The second heating element is configured to heat the first substrate via radiation.

[0210] Clause 24. A sintering furnace according to any clause or example herein, particularly the sintering furnace of Clause 23, wherein, in the fourth position, the spacing between the second heating element and the first substrate is in the range of 0-1 cm.

[0211] Clause 25. A sintering furnace according to any clause or example of this document, particularly a sintering furnace according to any of clauses 22 to 24, wherein the second heating element includes one or more displacement guides.

[0212] Clause 26. A sintering furnace according to any clause or example of this document, particularly the sintering furnace of Clause 25, wherein one or more displacement guides comprise refractory ceramics, or one or more displacement guides are formed of carbides.

[0213] Clause 27. A sintering furnace pursuant to any clause or example herein, particularly a sintering furnace pursuant to any of clauses 1 to 26, further includes:

[0214] The pressure plate inside the housing; and

[0215] Compression actuator, which is coupled to the pressure plate,

[0216] The control system is operatively coupled to the compression actuator, and a computer-readable storage medium stores additional instructions that, when executed by one or more processors, cause the control system to move the pressure plate via the compression actuator to press a first heating element of at least one heating element into the first substrate during step (b).

[0217] Clause 28. A sintering furnace according to any clause or example of this document, particularly the sintering furnace of Clause 27, wherein a compression actuator is disposed outside the housing and coupled to a pressure plate via one or more links.

[0218] Clause 29. A sintering furnace pursuant to any clause or example herein, particularly a sintering furnace pursuant to any of clauses 27 to 28, wherein:

[0219] The pressure plate includes refractory ceramics;

[0220] The pressure plate is formed of carbides;

[0221] One or more connecting rods include refractory ceramics;

[0222] One or more connecting rods are formed of carbides; or

[0223] Any combination of the above.

[0224] Clause 30. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 1 to 29, wherein the conveying assembly comprises one or more support rollers, one or more rotary actuators, a conveyor belt, or any combination of the foregoing components.

[0225] Clause 31. A sintering furnace pursuant to any clause or example herein, particularly a sintering furnace pursuant to Clause 30, also includes:

[0226] A pair of first current conductors, electrically coupled to opposite ends of a first heating element in at least one heating element;

[0227] A pair of second current conductors, electrically coupled at opposite ends to a conveyor belt in the heating region, wherein a portion of the conveyor belt in the heating region forms a second heating element in at least one heating element; or

[0228] Any combination of the above.

[0229] Clause 32. A sintering furnace pursuant to any clause or example herein, particularly a sintering furnace pursuant to any clause 31, wherein:

[0230] The first current conductor pair, the second current conductor pair, or both include refractory metal; or

[0231] The first current conductor pair, the second current conductor pair, or both are made of tungsten.

[0232] Clause 33. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 30 to 32, wherein a conveyor belt passes through and supports a first substrate within a heating zone.

[0233] Clause 34. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 30 to 33, wherein a first heating element of at least one heating element is spaced apart from a first substrate in a heating region, the first heating element being actuable between a third position away from the first substrate and a fourth position in contact with the first substrate, and configured to heat the first substrate via conduction.

[0234] Clause 35. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 30 to 34, wherein a first heating element of at least one heating element is spaced apart from a first substrate in a heating region, the first heating element being actuable between a third position away from the first substrate and a fourth position close to the first substrate, and configured to heat the first substrate by radiation.

[0235] Clause 36. A sintering furnace according to any clause or example herein, particularly the sintering furnace of Clause 35, wherein, in the fourth position, the spacing between the first heating element and the first substrate of at least one heating element is in the range of 0-1 cm.

[0236] Clause 37. A sintering furnace according to any clause or example herein, particularly any of clauses 1 to 36, further includes a cooling system thermally coupled to the shell and configured to cool the shell.

[0237] Clause 38. A sintering furnace according to any clause or example herein, particularly the sintering furnace of Clause 37, wherein the cooling system includes a heat exchanger through which at least one working fluid flows.

[0238] Clause 39. A sintering furnace according to any clause or example herein, particularly the sintering furnace of Clause 38, wherein at least one working fluid comprises water, air, oil, liquid nitrogen, or any combination thereof.

[0239] Clause 40. A sintering furnace according to any clause or example of this document, particularly a sintering furnace according to any of clauses 38 to 39, wherein the heat exchanger includes a meandering duct configured to be adjacent to or in contact with the shell of the shell.

[0240] Clause 41. A sintering furnace pursuant to any clause or example herein, particularly a sintering furnace pursuant to any of clauses 1 to 40, wherein:

[0241] The housing has one or more gas ports coupled to an inert gas source; and

[0242] The housing is configured such that inert gas supplied to one or more gas ports flows through the internal volume and exits via inlets and outlets.

[0243] Clause 42. A sintering furnace according to any clause or example of this document, particularly any of clauses 1 to 41, wherein the internal volume of the shell is at least 100 times larger than the size of the heating zone.

[0244] Clause 43. A sintering furnace pursuant to any clause or example herein, particularly a sintering furnace pursuant to any clause 41, further includes:

[0245] A first insulating layer, disposed within the internal volume and located between at least one heating element and the shell of the housing; and

[0246] The second insulating layer is disposed within the internal volume and is located between the shell of the transmission component and the housing.

[0247] Clause 44. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to Clause 43, wherein a first insulating layer, a second insulating layer, or both form one or more conduits extending from one or more gas ports and directing inert gas to a portion of a conveying assembly near the inlet, to a portion of a conveying assembly near the outlet, to a first end of at least one heating element, to a second end of at least one heating element, or to any combination of the aforementioned components.

[0248] Clause 45. A sintering furnace pursuant to any clause or example herein, particularly a sintering furnace pursuant to any of clauses 43 to 44, wherein:

[0249] The shell of the casing includes metal;

[0250] The shell of the casing is made of aluminum or stainless steel;

[0251] The first insulating layer, the second insulating layer, or both are formed of glass fiber or porous ceramic aerogel; or

[0252] Any combination of the above.

[0253] Clause 46. A sintering furnace pursuant to any clause or example herein, particularly a sintering furnace pursuant to any of clauses 41 to 45, further includes:

[0254] One or more protective gas baffles define an area where at least one heating element is disposed, and the one or more protective gas baffles define at least one conduit that directs inert gas from one or more gas ports to one or more ends of at least one heating element.

[0255] Clause 47. A sintering furnace according to any clause or example herein, particularly any of clauses 1 to 46, further includes one or more protective gas nozzles disposed within an internal volume and configured to direct gas flow to one or more ends of at least one heating element.

[0256] Clause 48. A sintering furnace pursuant to any clause or example herein, particularly a sintering furnace pursuant to any of clauses 1 to 47, further includes:

[0257] The first mechanical positioner is configured to load the substrate onto the transfer assembly near and upstream of the housing inlet;

[0258] A second mechanical positioner is configured to unload the substrate from the transfer assembly near and downstream of the housing outlet; or

[0259] Both of the above.

[0260] Clause 49. A sintering furnace pursuant to any clause or example herein, particularly a sintering furnace pursuant to any of clauses 1 to 48, further includes:

[0261] A dispenser configured to deposit one or more precursors onto a substrate supported by a transfer assembly or onto a substrate that is part of a transfer assembly at a location near and upstream of the housing inlet.

[0262] A sampler configured to receive one or more sintered materials from a substrate supported by a transfer assembly or from a substrate that is part of a transfer assembly, near and downstream of the housing outlet; or

[0263] Both of the above.

[0264] Clause 50. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 1 to 49, wherein one or more substrates include a portion of a transfer assembly.

[0265] Clause 51. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 1 to 50, wherein one or more substrates include a portion of a conveyor belt of a conveying assembly.

[0266] Clause 52. A sintering furnace according to any clause or example herein, particularly the sintering furnace of Clause 51, wherein the conveyor belt is formed of conductive carbon material.

[0267] Clause 53. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 1 to 52, wherein the first heating element of at least one heating element has a plan view of at least 20 cm. 2 The area.

[0268] Clause 54. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 1 to 53, wherein a computer-readable storage medium stores instructions that cause a control system to control at least one heating element, such that, when executed by one or more processors:

[0269] During the second time period immediately preceding the first time period, the temperature in the heated zone rose from approximately room temperature to the first temperature; and

[0270] During the third time period immediately following the first time period, the temperature in the heating zone drops from the first temperature to approximately room temperature.

[0271] Clause 55. Sintering furnaces according to any clause or example herein, particularly sintering furnaces according to Clause 54, wherein:

[0272] The duration of the second time period is longer than the duration of the first time period;

[0273] The duration of the second time period is 30 seconds or less;

[0274] The duration of the first time period is longer than the duration of the third time period;

[0275] The duration of the first time interval is approximately 10 seconds;

[0276] The duration of the third time period is 5 seconds or less;

[0277] The rate at which the temperature is heated to the first temperature during the second time period is less than the rate at which it is cooled from the first temperature during the third time period.

[0278] During the second time period, the rate of heating to the first temperature is at least 100°C / s;

[0279] During the third time period, the cooling rate from the first temperature is at least 100°C / s; or

[0280] Any combination of the above.

[0281] Clause 56. A sintering furnace comprising:

[0282] A shell that defines the internal volume, the inlet of the internal volume, and the outlet of the internal volume;

[0283] A dispenser for supplying one or more precursor particles to the inlet of the housing;

[0284] At least one heating element is disposed within the internal volume of the housing and located between the inlet and outlet, each heating element being configured to subject one or more precursor particles to a temperature profile; and

[0285] A control system operatively coupled to at least one heating element, the control system comprising one or more processors and a computer-readable storage medium storing instructions which, when executed by the one or more processors, cause the control system to bring one or more precursor particles to a first temperature of at least 500°C for a first time period via the at least one heating element.

[0286] Clause 57. A sintering furnace according to any clause or example herein, particularly the sintering furnace of Clause 56, wherein each heating element is porous, such that one or more precursor particles pass through the heating element when subjected to a first temperature.

[0287] Clause 58. A sintering furnace pursuant to any clause or example herein, particularly a sintering furnace pursuant to any of clauses 56 to 57, further includes:

[0288] The gas manifold connects to the distributor, the inert gas source, and the housing inlet.

[0289] The gas manifold is configured to combine one or more precursor particles with an inert gas flow, such that the one or more precursor particles are carried by the inert gas flow through at least one heating element.

[0290] Clause 59. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 56 to 58, further includes a sampler configured to receive one or more sintered particles from a shell outlet.

[0291] Clause 60. Sintering furnaces pursuant to any clause or example herein, particularly sintering furnaces pursuant to Clause 59, wherein:

[0292] The sampler is connected to the outlet of the housing; and

[0293] The sampler includes a porous filter membrane that allows an inert gas stream to pass through while capturing sintered particles on the inert gas stream.

[0294] Clause 61. A sintering furnace according to any clause or example of this document, particularly a sintering furnace according to any of clauses 56 to 60, wherein at least one heating element is electrically coupled to a current source via conductive paste.

[0295] Clause 62. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 56 to 61, wherein:

[0296] At least one heating element comprises a pair of substantially parallel heating elements separated by a gap, in order to define a vertically extending heating volume;

[0297] The distributor is positioned vertically above the inlet of the housing, allowing one or more precursor particles to be conveyed to the inlet and, under gravity, pass through a vertically extending heated volume; and

[0298] The sampler is positioned vertically below the outlet of the housing, allowing one or more sintered particles in the heating volume to pass through the outlet and reach the sampler under the influence of gravity.

[0299] Clause 63. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 56 to 62, wherein at least one heating element comprises a Joule heating element formed of carbon, graphite, metal or any combination of the above materials.

[0300] Clause 64. The sintering furnace according to any one of claims 56 to 63 further comprises:

[0301] Current source; and

[0302] An electrical wire that couples a current source to at least one heating element.

[0303] The control system is operatively coupled to the current source, and a computer-readable storage medium stores instructions that cause the control system to control the current source, which, when executed by one or more processors, cause the current source to apply current pulses to at least one heating element via wires, thereby subjecting one or more precursor particles to a first temperature.

[0304] Clause 65. A sintering furnace according to any clause or example herein, particularly the sintering furnace of Clause 64, wherein the wires comprise refractory metals or are formed of tungsten.

[0305] Clause 66. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 56 to 65, wherein:

[0306] The first temperature range is 1000 to 3000℃ (inclusive);

[0307] The duration of the first time period is less than or equal to 60 seconds;

[0308] The duration of the first time interval is approximately 10 seconds; or

[0309] Any combination of the above.

[0310] Clause 67. A sintering furnace according to any clause or example herein, particularly any of clauses 56 to 66, further includes a cooling system thermally coupled to the shell and configured to cool the shell.

[0311] Clause 68. A sintering furnace according to any clause or example herein, particularly the sintering furnace of Clause 67, wherein the cooling system includes a heat exchanger through which at least one working fluid flows.

[0312] Clause 69. A sintering furnace according to any clause or example herein, particularly the sintering furnace of Clause 68, wherein at least one working fluid comprises water, air, oil, liquid nitrogen, or any combination thereof.

[0313] Clause 70. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 68 to 69, wherein the heat exchanger includes a meandering duct configured to be adjacent to or in contact with the shell of the shell.

[0314] Clause 71. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to any of clauses 56 to 70, wherein a computer-readable storage medium stores instructions that cause a control system to control at least one heating element, such that, when executed by one or more processors:

[0315] During the second time period immediately preceding the first time period, the temperature in the heated zone rose from approximately room temperature to the first temperature; and

[0316] During the third time period immediately following the first time period, the temperature in the heating zone drops from the first temperature to approximately room temperature.

[0317] Clause 72. A sintering furnace according to any clause or example herein, particularly a sintering furnace according to Clause 71, wherein:

[0318] The duration of the second time period is longer than the duration of the first time period;

[0319] The duration of the second time period is 30 seconds or less;

[0320] The duration of the first time period is longer than the duration of the third time period;

[0321] The duration of the first time interval is approximately 10 seconds;

[0322] The duration of the third time period is 5 seconds or less;

[0323] The rate at which the temperature is heated to the first temperature during the second time period is less than the rate at which it is cooled from the first temperature during the third time period.

[0324] During the second time period, the rate of heating to the first temperature is at least 100°C / s;

[0325] During the third time period, the cooling rate from the first temperature is at least 100°C / s; or

[0326] Any combination of the above.

[0327] in conclusion

[0328] For example, regarding Figures 1A to 22 And any feature shown or described herein in Clauses 1 through 72 may be related to, for example, the features concerning Figures 1A to 22 Combined with any other features shown or described herein in Clauses 1 through 72, to provide systems, apparatus, methods, and embodiments not otherwise stated or specifically described herein. For example, Figures 4B to 4C The clip can be applied to Figures 1A to 1C as well as Figures 5A to 22 Any heating element in the system. In another example, Figures 8A to 8C and / or Figures 16A to 16C and / or Figures 18A to 18B The protective gas configuration can be applied to Figures 1A to 1C as well as Figures 5A to 22 Any furnace. Other combinations and variations are also possible depending on one or more intended embodiments. In fact, all features described herein are independent of each other and can be used in combination with any other feature described herein unless structurally impossible.

[0329] Given that the principles of the disclosed technology can be applied to many possible embodiments, it should be understood that the illustrated embodiments are merely examples and should not be considered as limiting the scope of the disclosed technology. Rather, the scope is defined by the following claims. Therefore, all rights falling within the scope and spirit of these claims are claimed herein.

Claims

1. A sintering furnace, comprising: A shell that defines the internal volume, the inlet of the internal volume, and the outlet of the internal volume; At least one heating element is disposed within the internal volume of the housing and located between the inlet and the outlet, each heating element being configured to subject the heated area to a temperature profile. A transfer assembly for moving one or more substrates into a housing, moving one or more substrates within a housing, and moving one or more substrates out of a housing; and A control system operably coupled to at least one heating element and a conveying assembly, the control system including one or more processors and a computer-readable storage medium storing instructions, which, when executed by the one or more processors, enable the control system to: (a) A first substrate having one or more precursors is moved through an inlet to a heating zone via a transfer assembly; (b) The first substrate in the heating zone is subjected to a first temperature of at least 500ºC during a first time period via at least one heating element; and (c) The first substrate having one or more sintered materials on it is removed from the heating zone via an outlet through a conveying assembly; The sintering furnace, for each heating element, further includes: A first conductive clamp is coupled to the first end of a corresponding heating element; A second conductive clamp is coupled to the second end of a corresponding heating element, the position of which is opposite to the position of the first end; A first metal clamp, coupled to the first conductive clamp, applies a clamping force to the first conductive clamp and the first end of the corresponding heating element; and A second metal clamp is coupled to the second conductive clamp and applies a clamping force to the second conductive clamp and the second end of the corresponding heating element.

2. The sintering furnace according to claim 1, wherein at least one heating element comprises a Joule heating element, said Joule heating element being formed of carbon, graphite, metal or any combination of the above materials.

3. The sintering furnace according to claim 1, wherein at least one heating element is formed as a sheet or film.

4. The sintering furnace according to claim 1, wherein: The first conductive clamp, the second conductive clamp, or both may include one or more graphite plates; The first metal clip, the second metal clip, or both of them include a copper clip or a stainless steel clip with a copper coating; or any combination thereof.

5. The sintering furnace according to claim 1, further comprising: Current source; and The wire couples the current source to the first metal clip and the second metal clip. The control system is operatively coupled to the current source, and a computer-readable storage medium stores instructions that cause the control system to control the current source, which, when executed by one or more processors, cause the current source to apply current pulses to at least one heating element via wires, thereby subjecting the first substrate to a first temperature.

6. The sintering furnace according to claim 5, wherein the wire comprises a refractory metal, or the wire is formed of tungsten.

7. The sintering furnace according to claim 1, wherein: The ratio of the travel length between the inlet and outlet within the casing to the length of the heating zone is at least 100:1; The ratio of the internal volume to the volume of the heating zone is at least 100:1; or Both of the above.

8. The sintering furnace according to claim 7, wherein: The ratio of the travel length to the length of the heating area ranges from 100:1 to 1000:1, including 100:1 and 1000:1; The ratio of the internal volume to the volume of the heating zone ranges from 100:1 to 1000:1, including 100:1 and 1000:1; or Both of the above.

9. The sintering furnace according to claim 1, wherein: The first temperature range is 1000 to 3000°C, including 1000°C and 3000°C; The duration of the first time period is less than or equal to 60 seconds; The duration of the first time interval is approximately 10 seconds; At the start of the first time period, the heating slope to reach the first temperature is at least 10. 2 ℃ / s; At the end of the first time period, the cooling slope from the first temperature is at least 10. 3 ℃ / s, or; Any combination of the above.

10. The sintering furnace according to claim 1, wherein: The first substrate comprises a polymer; and A computer-readable storage medium stores additional instructions that, when executed by one or more processors, cause the control system to proceed prior to step (b): (d) The first substrate is subjected to a temperature lower than 10℃ via at least one heating element or another heating element within the housing. The first temperature is used to carbonize the polymer on the first substrate.

11. The sintering furnace according to claim 1, wherein: The first substrate comprises a polymer; and A computer-readable storage medium stores additional instructions that, when executed by one or more processors, cause the control system to proceed prior to step (a): (d) Carbonizing the polymer of the first substrate by subjecting the first substrate to a temperature lower than a first temperature via at least one external heating element.

12. The sintering furnace according to any one of claims 10 to 11, wherein the temperature in step (d) is below 200°C.

13. The sintering furnace according to any one of claims 10 to 11, wherein the duration of the time period in step (d) is greater than the duration of the first time period in step (b).

14. The sintering furnace of claim 1, wherein the conveying assembly comprises one or more support rollers, one or more conveying rollers, one or more rotary actuators, a conveyor belt, or any combination of the foregoing components.

15. The sintering furnace of claim 14, wherein the conveying assembly comprises: One or more first conveyor rollers are disposed before the heating zone and configured to separate the first substrate from the conveyor belt and convey the first substrate to the heating zone; and One or more second transfer rollers are disposed after the heating zone and configured to transfer the first substrate from the heating zone to the conveyor belt.

16. The sintering furnace according to claim 15, wherein the conveyor belt passes around or below the heating zone.

17. The sintering furnace according to claim 14, wherein: One or more support rollers comprise one or more metals; One or more support rollers are made of stainless steel; One or more conveyor rollers comprise one or more refractory metals; One or more conveyor rollers are made of tungsten; The conveyor belt is made of carbon; or Any combination of the above.

18. The sintering furnace according to claim 14, wherein: At least one heating element includes a first heating element disposed in a heating region to support a first substrate, the first heating element being configured to heat the first substrate via conduction.

19. The sintering furnace of claim 18, further comprising a transfer actuator configured to move a first heating element between a first position and a second position, the first position supporting a first substrate in a substantially horizontal direction, the second position being angled relative to the horizontal direction such that the first substrate slides from the heating region.

20. The sintering furnace according to claim 19, wherein: The transmission actuator includes refractory ceramics; or The transmission actuator is made of carbide.

21. The sintering furnace according to claim 14, wherein: At least one heating element includes a second heating element spaced apart from the first substrate in the heating region; The second heating element can be actuated between a third position away from the first substrate and a fourth position in contact with the first substrate; and The second heating element is configured to heat the first substrate via conduction.

22. The sintering furnace according to claim 14, wherein: At least one heating element includes a second heating element spaced apart from the first substrate in the heating region; The second heating element can be actuated between a third position away from the first substrate and a fourth position close to the first substrate; and The second heating element is configured to heat the first substrate via radiation.

23. The sintering furnace according to claim 22, wherein, In the fourth position, the distance between the second heating element and the first substrate is in the range of 0-1 cm.

24. The sintering furnace according to any one of claims 21 to 23, wherein the second heating element comprises one or more displacement guides.

25. The sintering furnace according to claim 24, wherein: One or more displacement guides include refractory ceramics; or One or more displacement guides are formed of carbides.

26. The sintering furnace according to claim 1, further comprising: Pressure plates inside the housing; and Compression actuator, which is coupled to the pressure plate, The control system is operatively coupled to the compression actuator, and a computer-readable storage medium stores additional instructions that, when executed by one or more processors, cause the control system to move the pressure plate via the compression actuator to press a first heating element of at least one heating element into the first substrate during step (b).

27. The sintering furnace of claim 26, wherein the compression actuator is disposed outside the housing and coupled to the pressure plate via one or more connecting rods.

28. The sintering furnace according to claim 27, wherein: The pressure plate includes refractory ceramics; The pressure plate is formed of carbides; One or more connecting rods include refractory ceramics; One or more connecting rods are formed of carbides; or Any combination of the above.

29. The sintering furnace of claim 1, wherein the conveying assembly comprises one or more support rollers, one or more rotary actuators, a conveyor belt, or any combination of the foregoing components.

30. The sintering furnace according to claim 29, further comprising: A pair of first current conductors, electrically coupled to opposite ends of a first heating element in at least one heating element; A pair of second current conductors, electrically coupled at opposite ends to a conveyor belt in the heating region, wherein a portion of the conveyor belt in the heating region forms a second heating element in at least one heating element; or Any combination of the above.

31. The sintering furnace according to claim 30, wherein: The first current conductor pair, the second current conductor pair, or both include refractory metal; or The first current conductor pair, the second current conductor pair, or both are made of tungsten.

32. The sintering furnace of claim 29, wherein the conveyor belt passes through and supports the first substrate within the heating area.

33. The sintering furnace of claim 30, wherein a first heating element of at least one heating element is spaced apart from a first substrate in a heating region, the first heating element being actuable between a third position away from the first substrate and a fourth position in contact with the first substrate, and configured to heat the first substrate via conduction.

34. The sintering furnace of claim 30, wherein a first heating element of at least one heating element is spaced apart from a first substrate in a heating region, the first heating element being actuable between a third position away from the first substrate and a fourth position close to the first substrate, and configured to heat the first substrate via radiation.

35. The sintering furnace according to claim 34, wherein, In the fourth position, the distance between the first heating element and the first substrate in at least one heating element is in the range of 0-1 cm.

36. The sintering furnace according to claim 1 further includes a cooling system, the cooling system being thermally coupled to the shell and configured to cool the shell.

37. The sintering furnace of claim 36, wherein the cooling system includes a heat exchanger through which at least one working fluid flows.

38. The sintering furnace according to claim 37, wherein at least one working fluid comprises water, air, oil, liquid nitrogen, or any combination thereof.

39. The sintering furnace according to claim 37, wherein the heat exchanger includes a meandering duct, the meandering duct being configured to be adjacent to or in contact with the shell of the shell.

40. The sintering furnace according to claim 1, wherein: The housing has one or more gas ports coupled to an inert gas source; and The housing is configured such that inert gas supplied to one or more gas ports flows through the internal volume and exits via inlets and outlets.

41. The sintering furnace according to claim 40, wherein the internal volume of the shell is at least 100 times larger than the size of the heating zone.

42. The sintering furnace according to claim 40, further comprising: A first insulating layer is disposed within the internal volume and located between at least one heating element and the shell of the housing; and The second insulating layer is disposed within the internal volume and is located between the conveying assembly and the housing shell.

43. The sintering furnace of claim 42, wherein the first insulating layer, the second insulating layer, or both form one or more conduits extending from one or more gas ports and directing inert gas to a portion of the conveying assembly near the inlet, to a portion of the conveying assembly near the outlet, to a first end of at least one heating element, to a second end of at least one heating element, or to any combination thereof.

44. The sintering furnace according to claim 42, wherein: The shell of the casing includes metal; The shell of the casing is made of aluminum or stainless steel; The first insulating layer, the second insulating layer, or both are formed of glass fiber or porous ceramic aerogel; or any combination thereof.

45. The sintering furnace according to claim 40, further comprising: One or more protective gas baffles define an area where at least one heating element is disposed, and the one or more protective gas baffles define at least one conduit that directs inert gas from one or more gas ports to one or more ends of at least one heating element.

46. ​​The sintering furnace according to claim 1, further comprising: One or more protective gas nozzles are disposed within an internal volume and configured to direct airflow to one or more ends of at least one heating element.

47. The sintering furnace according to claim 1, further comprising: The first mechanical positioner is configured to load the substrate onto the transfer assembly near and upstream of the housing inlet; A second mechanical positioner is configured to unload the substrate from the transfer assembly near and downstream of the housing outlet; or Both of the above.

48. The sintering furnace according to claim 1, further comprising: A dispenser configured to deposit one or more precursors onto a substrate supported by a transfer assembly or onto a substrate that is part of a transfer assembly at a location near and upstream of the housing inlet. A sampler configured to receive one or more sintered materials from a substrate supported by a transfer assembly or from a substrate that is part of a transfer assembly, near and downstream of the housing outlet; or Both of the above.

49. The sintering furnace of claim 1, wherein one or more substrates include a portion of a conveying assembly.

50. The sintering furnace of claim 1, wherein one or more substrates include a portion of a conveyor belt of a conveying assembly.

51. The sintering furnace according to claim 50, wherein the conveyor belt is formed of a conductive carbon material.

52. The sintering furnace according to claim 1, wherein the first heating element of at least one heating element has a planar area of ​​at least 20 cm. 2 The area.

53. The sintering furnace of claim 1, wherein the computer-readable storage medium stores instructions that cause the control system to control at least one heating element, wherein when the instructions are executed by one or more processors, the following are caused: During the second time period immediately preceding the first time period, the temperature in the heated zone rose from approximately room temperature to the first temperature; and During the third time period immediately following the first time period, the temperature in the heating zone drops from the first temperature to approximately room temperature.

54. The sintering furnace according to claim 53, wherein: The duration of the second time period is longer than the duration of the first time period; The duration of the second time period is 30 seconds or less; The duration of the first time period is longer than the duration of the third time period; The duration of the first time interval is approximately 10 seconds; The duration of the third time period is 5 seconds or less; The rate at which the temperature is heated to the first temperature during the second time period is less than the rate at which it is cooled from the first temperature during the third time period. During the second time period, the rate of heating to the first temperature is at least 100°C / s; During the third time period, the cooling rate from the first temperature is at least 100°C / s; or Any combination of the above.

55. A sintering furnace, comprising: A shell that defines the internal volume, the inlet of the internal volume, and the outlet of the internal volume; A dispenser for supplying one or more precursor particles to the inlet of the housing; At least one heating element is disposed within the internal volume of the housing and located between the inlet and the outlet, each heating element being configured to subject one or more precursor particles to a temperature profile. A sampler configured to receive one or more sintered particles from the outlet of the housing; and A control system operatively coupled to at least one heating element, the control system including one or more processors and a computer-readable storage medium storing instructions which, when executed by the one or more processors, cause the control system to subject one or more precursor particles to a first temperature of at least 500°C for a first time period via the at least one heating element. Each heating element is porous, allowing one or more precursor particles to pass through the heating element when subjected to a first temperature.

56. The sintering furnace according to claim 55, further comprising: The gas manifold connects to the distributor, the inert gas source, and the housing inlet. The gas manifold is configured to combine one or more precursor particles with an inert gas flow, such that the one or more precursor particles are carried by the inert gas flow through at least one heating element.

57. The sintering furnace according to claim 56, wherein: The sampler is connected to the outlet of the housing; and The sampler includes a porous filter membrane that allows an inert gas stream to pass through while capturing sintered particles on the inert gas stream.

58. The sintering furnace according to claim 55, wherein at least one heating element is electrically coupled to a current source via conductive adhesive.

59. The sintering furnace according to claim 55, wherein: At least one heating element comprises a pair of substantially parallel heating elements separated by a gap, in order to define a vertically extending heating volume; The distributor is positioned vertically above the inlet of the housing, allowing one or more precursor particles to be fed into the inlet and pass through the vertically extending heated volume under gravity. and The sampler is positioned vertically below the outlet of the housing, allowing one or more sintered particles in the heating volume to pass through the outlet and reach the sampler under gravity.

60. The sintering furnace according to any one of claims 55 to 59, wherein at least one heating element comprises a Joule heating element formed of carbon, graphite, metal or any combination of the above materials.

61. The sintering furnace according to any one of claims 55 to 59, further comprising: Current source; and An electrical wire that couples a current source to at least one heating element. The control system is operatively coupled to the current source, and a computer-readable storage medium stores instructions that cause the control system to control the current source, which, when executed by one or more processors, cause the current source to apply current pulses to at least one heating element via wires, thereby subjecting one or more precursor particles to a first temperature.

62. The sintering furnace according to claim 61, wherein the wire comprises a refractory metal, or the wire is formed of tungsten.

63. The sintering furnace according to claim 55, wherein: The first temperature range is 1000 to 3000°C, including 1000°C and 3000°C; The duration of the first time period is less than or equal to 60 seconds; The duration of the first time interval is approximately 10 seconds; or Any combination of the above.

64. The sintering furnace according to claim 55 further includes a cooling system thermally coupled to the shell and configured to cool the shell.

65. The sintering furnace according to claim 64, wherein the cooling system includes a heat exchanger through which at least one working fluid flows.

66. The sintering furnace according to claim 65, wherein at least one working fluid comprises water, air, oil, liquid nitrogen, or any combination thereof.

67. The sintering furnace according to claim 65, wherein the heat exchanger includes a meandering duct, the meandering duct being configured to be adjacent to or in contact with the shell of the shell.

68. The sintering furnace of claim 55, wherein the computer-readable storage medium stores instructions that cause the control system to control at least one heating element, such that, when the instructions are executed by one or more processors: During the second time period immediately preceding the first time period, the temperature in the heated zone rose from approximately room temperature to the first temperature; and During the third time period immediately following the first time period, the temperature in the heating zone drops from the first temperature to approximately room temperature.

69. The sintering furnace according to claim 68, wherein: The duration of the second time period is longer than the duration of the first time period; The duration of the second time period is 30 seconds or less; The duration of the first time period is longer than the duration of the third time period; The duration of the first time interval is approximately 10 seconds; The duration of the third time period is 5 seconds or less; The rate at which the temperature is heated to the first temperature during the second time period is less than the rate at which it is cooled from the first temperature during the third time period. During the second time period, the rate of heating to the first temperature is at least 100°C / s; During the third time period, the cooling rate from the first temperature is at least 100°C / s; or Any combination of the above.

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