Device and method for batch production of silicon nitride nanowire flexible ceramic films

Abstract

The invention discloses a device and a method for batch production of silicon nitride nanowire flexible ceramic films, and belongs to the technical field of silicon nitride nanowire flexible ceramic films. The device comprises a box-type furnace body, an open space is formed in the bottom of the box-type furnace body, and a lifting table is installed in the open space; a detachable reaction chamber formed by splicing a plurality of brick bodies is supported above the lifting table, and a graphite mold is arranged in the reaction chamber; the inner wall of the box-type furnace body and the outer wall of the reaction chamber are arranged next to each other, a plurality of air inlet holes and air inlets which are arranged in an array manner are respectively formed in the side walls of the same sides of the box-type furnace body and the reaction chamber, the air inlet holes correspond to the air inlets, a plurality of air outlet holes and air outlets which are vertically arranged are respectively formed in the side walls of the opposite sides of the box-type furnace body and the reaction chamber, and the air outlet holes are aligned with the air outlets. The method is used for solving the technical problem that the yield of the existing silicon nitride nanowire flexible ceramic thin film is small.

Description

Technical Field

[0001] The present invention belongs to the technical field of silicon nitride nanowire flexible ceramic films, and in particular relates to a device and method for batch production of silicon nitride nanowire flexible ceramic films. Background Art

[0002] Silicon nitride ceramic nanowires, with their outstanding oxidation resistance, good corrosion resistance, and excellent high-temperature performance, exhibit remarkable advantages in thermal stability and thermal insulation properties, and have broad application prospects in aerospace thermal protection systems, high-temperature filtration materials, and high-temperature insulation materials. Currently, methods for preparing flexible ceramic films made of silicon nitride nanowires primarily include chemical vapor deposition (CVD), carbothermal reduction, and direct nitridation. Chinese invention patent publication number CN118083923A discloses a method for mass-producing silicon nitride nanowires by directly reacting solid-phase silicon sources SiO2 and Si with N2 via carbothermal reduction or direct nitridation to produce silicon nitride. During the preparation process, carbon paper is folded into a wavy shape to assist in controlling the nucleation and growth of silicon nitride. Cyclic charging and degassing is used to generate an oscillating N2 pressure to regulate the reaction process. This preparation method primarily utilizes the wavy carbon paper to promote the preferential growth of silicon nitride nanowires, and the constant regulation of N2 pressure is required. The experimental process is complex and cumbersome, making it difficult to develop a process specification, and the product is uneven.

[0003] However, the existing technology has the following problems: First, the existing devices for producing silicon nitride nanowire flexible ceramic films often use small tubular furnaces. Due to the limited size of their cavity, the output of the films is extremely limited, making it difficult to meet the needs of industrial production; second, the limitation of the cavity size of the tubular furnace makes the maximum area of the prepared films far smaller than the square meter size required for aerospace thermal protection components, which cannot meet the needs of actual applications; in addition, laboratory process parameters (such as heating rate and gas flow) may become unstable during the scale-up process, resulting in uncontrolled product output, affecting the consistency and reliability of product quality.

[0004] Therefore, there is an urgent need to develop a device that can mass-produce large-area silicon nitride nanowire flexible ceramic films to solve the problems of low yield, small format, and unstable process parameters in the existing technology. Summary of the Invention

[0005] In order to overcome the above-mentioned shortcomings of the prior art, the purpose of the present invention is to provide an apparatus and method for mass production of silicon nitride nanowire flexible ceramic films, so as to solve the technical problem of low output of the existing silicon nitride nanowire flexible ceramic films.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions: On the one hand, the present invention provides a device for batch production of silicon nitride nanowire flexible ceramic films, including a box-type furnace body, an open space is provided at the bottom of the box-type furnace body, and a lifting platform is installed inside the open space; a detachable reaction chamber composed of multiple bricks is supported above the lifting platform, and a graphite mold is placed inside the reaction chamber; the inner wall of the box-type furnace body is arranged closely to the outer wall of the reaction chamber, and a plurality of air inlets and air inlets arranged in an array are respectively provided on the side walls on the same side of the two, and the air inlets and air inlets correspond to each other, and a plurality of vertically arranged air outlets and air outlets are respectively provided on the side walls on the other side, and the air outlets and air outlets are aligned.

[0007] Furthermore, it includes a box-type furnace body, a lifting platform, a reaction chamber, an open space, an air inlet, an air outlet and a graphite mold placed in the reaction chamber, the graphite mold is in the reaction chamber during the production process to hold materials; the open space is arranged at the bottom of the box-type furnace body, the lifting platform is arranged at the bottom of the box-type furnace body, and the lifting platform is inside the open space; the reaction chamber is composed of a number of bricks, the reaction chamber can be disassembled to put in raw materials or take out products, and the reaction chamber is arranged above the lifting platform; the inner wall of the box-type furnace body and the outer wall of the reaction chamber are arranged closely, and a number of array-arranged air inlets and air outlets are respectively opened on the side wall on the same side of the box-type furnace body and the reaction chamber, and the air inlets and air outlets are aligned, and a number of vertically arranged air outlets and air outlets are respectively opened on the side wall on the other side, and the air outlets and air outlets are aligned.

[0008] In one embodiment, the reaction chamber is composed of a plurality of alumina ceramic bricks joined in a mortise and tenon manner, and the brick body of the reaction chamber can be optionally alumina ceramic bricks; the graphite mold includes a bearing plate and four sets of limit blocks arranged at the four corners of the bearing plate.

[0009] In one embodiment, a heating mechanism is provided on the inner wall of the reaction chamber, and the heating mechanism can be a silicon molybdenum rod (MoSi2). A control panel is provided on the outside of the box-type furnace body, and the control panel is electrically connected to the heating mechanism for controlling the temperature inside the reaction chamber.

[0010] In one embodiment, the air inlet holes and the air inlet ports are connected to several groups of air inlet pipes, the air inlet pipes are arranged on an air pipe rack, and the inlets of the air inlet pipes are connected to an air source; the air inlet pipes are connected to an air pump, and a flow meter is arranged on the air inlet pipes, and the flow meter is used to control the intake flow.

[0011] In one embodiment, the open space is a space formed by a cubic frame; and the lifting platform is an electric push rod lifting platform consisting of a table top and a lifting rod located in the middle of the table top.

[0012] In one embodiment, the air outlet is connected to several tail gas bottles; the apertures of the air inlet and the air inlet are equal, the apertures of the air outlet and the air outlet are equal, and the apertures of the air inlet and the air inlet are smaller than the apertures of the air outlet and the air outlet.

[0013] The present invention also provides a method for batch production of silicon nitride nanowire flexible ceramic films, which uses the above-mentioned device for batch production of silicon nitride nanowire flexible ceramic films, characterized by comprising the following steps: A mixed powder of silicon dioxide and carbon nanotubes is placed in a graphite mold. Graphite paper is cut to match the size of the graphite mold and covered over the mixed powder in the graphite mold. A lifting platform lowers the reaction chamber to an open space, and multiple graphite molds are stacked in the reaction chamber. The reaction chamber is then raised to the furnace body of the box-type furnace. Start the box-type furnace, adjust the flow rate of nitrogen, raise the temperature of the reaction chamber to the set temperature, introduce nitrogen into the reaction chamber through the air inlet and air inlet to react with the mixed powder in the gas phase, and then discharge it through the air outlet and air outlet; After the reaction is completed, the reaction chamber is cooled to room temperature, and the lifting platform drives the reaction chamber down to the open space, the graphite paper is taken out, and the product on the graphite paper is collected to obtain a silicon nitride nanowire flexible ceramic film.

[0014] In one embodiment, the set temperature is 1450-1550° C.; and the gas phase reaction time is 3-6 hours.

[0015] In one embodiment, the nitrogen flow rate introduced into each of the air inlet holes and the air inlet is 0.5-2 L / min.

[0016] In one embodiment, the temperature of the temperature-elevated reaction chamber is increased at a rate of 3-10° C. / min.

[0017] Compared with the prior art, the present invention has the following beneficial effects: The present invention provides a device for batch production of silicon nitride nanowire flexible ceramic films. By adopting a box-type furnace body to replace the traditional small tube furnace, the space utilization rate of the reaction chamber is greatly improved, and multiple graphite molds can be placed at the same time for batch production, which significantly increases the output of silicon nitride nanowire flexible ceramic films. The reaction chamber of the present invention is composed of a plurality of brick bodies, which can be disassembled to form an open structure to realize the removal of materials and can produce square meter-level films that meet the requirements of aerospace thermal protection components. The design of the lifting platform facilitates the loading and unloading of the reaction chamber and the placement and removal of raw materials and products, thereby improving production efficiency. The reasonable design of the air inlet, air inlet and air outlet ensures the uniform distribution of the reaction gas in the chamber, which is conducive to improving the consistency of product quality.

[0018] Furthermore, by setting up a control panel electrically connected to the heating mechanism and setting a flow meter on the air inlet pipe, precise control of the reaction temperature and gas flow is achieved, ensuring the stability of the process parameters and making the product output controllable.

[0019] The present invention also provides a method for mass-producing silicon nitride nanowire flexible ceramic thin films. This method utilizes a vapor phase process. Using the aforementioned apparatus for mass-producing silicon nitride nanowire flexible ceramic thin films, an atmosphere box furnace can be used to heat-treat multiple layers of raw materials in a single step to produce the silicon nitride nanowire thin films, thereby reducing production costs and providing a foundation for mass production. The silicon nitride flexible ceramic thin films produced using the vapor phase process exhibit uniformity, good crystallinity, high purity, superior quality, and minimal environmental pollution. Furthermore, the method is simple to operate, economical and convenient, and features a clean, pollution-free preparation process, making it easy to operate. This method has significant research value and broad application prospects in various fields. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 A schematic diagram of a device for mass production of silicon nitride nanowire flexible ceramic films provided by the present invention; Figure 2 A cross-sectional view of a device for batch production of silicon nitride nanowire flexible ceramic films provided by the present invention; Figure 3 A schematic diagram of a method for mass production of silicon nitride nanowire flexible ceramic films provided by the present invention; Figure 4 It is a structural schematic diagram of the graphite mold of the present invention; Figure 5 This is a scanning electron micrograph of a silicon nitride nanowire flexible ceramic film produced by reducing industrial-grade silicon dioxide powder and carbon nanotube powder in an apparatus for mass production of silicon nitride nanowire flexible ceramic films according to Example 1 of the present invention; Figure 6 This is a photograph of the silicon nitride nanowire flexible ceramic film prepared in Example 1 of the present invention; Figure 7 This is a photograph of the silicon nitride nanowire flexible ceramic film prepared in Example 2 of the present invention; Figure 8 This is a photograph of the silicon nitride nanowire flexible ceramic film prepared in Example 3 of the present invention; Figure 9 This is a photograph of the silicon nitride nanowire flexible ceramic film prepared in Example 4 of the present invention; Figure 10 This is a photograph of the silicon nitride nanowire flexible ceramic film prepared in Example 5 of the present invention; Figure 11 This is a photograph of the silicon nitride nanowire flexible ceramic film prepared in Example 6 of the present invention; Figure 12 This is a photo of the silicon nitride nanowire flexible ceramic film prepared in Example 7 of the present invention.

[0021] Among them: 1-box furnace body; 2-lifting platform; 3-control panel; 4-alumina ceramic brick; 5-air inlet; 6-air outlet; 7-air inlet. DETAILED DESCRIPTION

[0022] To facilitate understanding of the features and effects of the present invention by those skilled in the art, the following provides a general description and definition of the terms and expressions used in the specification and claims. Unless otherwise indicated, all technical and scientific terms used herein have the ordinary meanings as understood by those skilled in the art regarding the present invention. In the event of conflict, the definitions in this specification shall prevail.

[0023] The theories or mechanisms described and disclosed herein, whether correct or incorrect, should not limit the scope of the present invention in any way, that is, the present invention can be implemented without being limited by any specific theory or mechanism.

[0024] It should be noted that the terms "first", "second", etc. in the description and claims of the present invention and the above-mentioned drawings are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that the numbers used in this way can be interchanged where appropriate, so that the embodiments of the present invention described herein can be implemented in an order other than those illustrated or described herein. In addition, the terms "including" and "having" and any variations thereof are intended to cover non-exclusive inclusions. For example, a process, method, system, product or device that includes a series of steps or units is not necessarily limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products or devices.

[0025] All features, such as values, amounts, contents, and concentrations, described herein as numerical ranges or percentage ranges are provided for simplicity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to include and specifically disclose all possible subranges and individual values within the range (including integers and fractions).

[0026] In this document, for the sake of brevity, not all possible combinations of the various technical features in each embodiment or example are described. Therefore, as long as there are no contradictions in the combination of these technical features, the various technical features in each embodiment or example can be combined in any way, and all possible combinations should be considered to be within the scope of this specification.

[0027] The present invention provides a device and method for batch producing silicon nitride nanowire flexible ceramic films.

[0028] See also Figure 1 and Figure 2 In the first aspect, a device for batch production of silicon nitride nanowire flexible ceramic films is provided, which includes a box-type furnace body 1, a lifting platform 2, a reaction chamber, an open space, an air inlet 5, an air outlet 6, an air inlet 7 and a graphite mold placed in the reaction chamber; the open space is arranged at the bottom of the box-type furnace body 1, and the lifting platform 2 is arranged at the bottom of the box-type furnace body 1, and the lifting platform 2 is inside the open space; the reaction chamber is composed of a plurality of bricks, and the reaction chamber can be disassembled to put in raw materials or take out products, and the reaction chamber is arranged above the lifting platform 2; the inner wall of the box-type furnace body 1 and the outer wall of the reaction chamber are arranged closely, and a plurality of air inlets 7 and air inlets 5 arranged in an array are respectively provided on the side walls on the same side of the box-type furnace body 1 and the reaction chamber, and the air inlet 7 and the air inlet 5 are aligned, and a plurality of vertically arranged air outlets 6 and the air outlet are respectively provided on the side walls on the opposite side, and the air outlet 6 and the air outlet are aligned.

[0029] More specifically, an open space is located at the bottom of the box-type furnace body 1. This open space, constructed from a cubical frame, provides ample space for loading and unloading the reaction chamber. A lifting platform 2 is located at the bottom of the box-type furnace body 1, within the open space. Lifting platform 2 is an electric push-rod platform consisting of a tabletop and a lifting rod located in the middle of the tabletop. The electric push-rod controls the height of lifting platform 2.

[0030] The reaction chamber is constructed from a number of bricks, preferably alumina ceramic bricks 4, joined together in a mortise and tenon-jointed pattern. Alumina ceramic bricks 4 exhibit excellent high-temperature resistance and chemical stability, maintaining structural stability in high-temperature reaction environments. The mortise and tenon-jointed structure ensures the reaction chamber's sealing and structural stability, while also facilitating its disassembly for loading raw materials or removing products. The reaction chamber is positioned above a lift platform 2, which allows for adjustment of its position.

[0031] The inner wall of the box-type furnace body 1 and the outer wall of the reaction chamber are positioned in close proximity to ensure uniform nitrogen flow. A plurality of inlet holes 7 and an inlet port 5 are arranged in an array on one side wall of the box-type furnace body 1 and the reaction chamber, respectively. The inlet holes 7 and the inlet port 5 are aligned to facilitate uniform entry of the reaction gas. A plurality of vertically arranged outlet holes 6 and an outlet port 5 are also provided on the opposite side wall, aligned to allow the reaction gas to be discharged.

[0032] Several sets of inlet pipes are connected to the inlet port 7 and the inlet port 5. These inlet pipes are mounted on a pipe rack. The inlet pipes are connected to a gas source to provide the gases required for the reaction. An air pump is connected to the inlet pipes to control the flow and pressure of the gas. A flow meter is installed on the inlet pipes to control the inlet flow rate and ensure accurate supply of the reaction gases. Several exhaust bottles are connected to the outlet port 7 to collect and process the exhaust gases generated during the reaction.

[0033] The apertures of the air inlet 7 and the air inlet 5 are equal, the apertures of the air outlet 6 and the air outlet are equal, and the apertures of the air inlet 7 and the air inlet 5 are smaller than the apertures of the air outlet 6 and the air outlet. This design ensures smooth flow of the reaction gas in the reaction chamber and prevents pressure accumulation due to obstruction of gas flow.

[0034] A heating mechanism is installed on the inner wall of the reaction chamber to provide the high temperature environment required for the reaction. A control panel 3 is installed on the outside of the box furnace body. The control panel is electrically connected to the heating mechanism and is used to control the temperature inside the reaction chamber to achieve precise control of the reaction process.

[0035] The graphite mold is placed in the reaction chamber to support the raw silicon dioxide and carbon nanotubes and the formed silicon nitride nanowire flexible ceramic film. Figure 4 The graphite mold consists of a carrier plate and four sets of L-shaped limit blocks at its four corners. The carrier plate is used to place the reaction raw materials, and the L-shaped limit blocks are used to define the shape and size of the formed silicon nitride nanowire flexible ceramic film, ensuring product consistency and specifications.

[0036] The working process of this device is as follows: First, the reaction chamber is disassembled in an open space, and a graphite mold containing raw materials is placed in it, and then the reaction chamber is reassembled and sealed. The reaction chamber is raised to an appropriate position by the lifting platform 2 so that the inner wall of the box furnace body 1 and the outer wall of the reaction chamber are in close contact. Start the control panel 3, set the reaction temperature, and heat the reaction chamber by the heating mechanism. At the same time, the reaction gas is introduced into the reaction chamber through the air inlet pipe, and the gas enters the reaction chamber through the air inlet 7 and the air inlet 5. The gas after the reaction is discharged through the air outlet 6 and the air outlet and is collected in the tail gas bottle. After the reaction is completed, the heating mechanism and the gas source are turned off. After the reaction chamber cools down, the reaction chamber is lowered by the lifting platform 2, the reaction chamber is disassembled, and the finished silicon nitride nanowire flexible ceramic film in the graphite mold is taken out.

[0037] Through a rational structural design and precise control system, this device achieves mass production of silicon nitride nanowire flexible ceramic films, characterized by high production efficiency and stable product quality. The detachable design of the reaction chamber facilitates the loading of raw materials and the removal of products. The provision of a lifting platform 2 simplifies the operating process and improves production efficiency. The design of the air inlet and outlet systems ensures the uniform distribution and smooth flow of the reaction gases, which is conducive to the full progress of the reaction. The combination of the heating mechanism and the control panel 3 enables precise control of the reaction temperature, ensuring the stability of product quality. The design of the graphite mold ensures the consistency of product specifications and meets the requirements of mass production.

[0038] Further preferably, the reaction chamber is constructed of zirconia ceramic tiles, with the reaction chamber formed by a plurality of zirconia ceramic tiles interlocked in a mortise and tenon arrangement. The graphite mold includes a support plate and four sets of T-shaped limit blocks positioned at the four corners of the support plate. Zirconia ceramic tiles have higher heat resistance and mechanical strength than alumina ceramic tiles, making them suitable for higher-temperature reaction environments. T-shaped limit blocks offer better positioning and greater stability than L-shaped limit blocks, enabling more precise control of the shape and size of the silicon nitride nanowire flexible ceramic film.

[0039] Further preferably, the air inlet hole 7 and the air inlet port 5 are connected with six or more groups of air inlet pipes, the air inlet pipes are arranged on an air pipe rack with adjustable height, and the inlet of the air inlet pipes is connected to a mixed gas source; a digital air pump is connected to the air inlet pipe, and an electronic flow meter is arranged on the air inlet pipe, which is connected to the control panel 3 for real-time monitoring and adjustment of the intake flow.

[0040] Multiple inlet pipes ensure uniform gas supply, while an adjustable-height gas pipe rack accommodates reaction chambers of varying heights. The mixed gas source provides a variety of gas mixtures to meet diverse reaction conditions. A digital gas pump and electronic flowmeter enhance the accuracy of gas flow control. Connection to the control panel 3 enables real-time monitoring and automatic adjustment of gas flow.

[0041] See also Figure 3 The second aspect of the present invention provides a method for mass producing silicon nitride nanowire flexible ceramic films using the above-mentioned apparatus for mass producing silicon nitride nanowire flexible ceramic films, comprising the following steps: S1: Place a mixed powder of silicon dioxide and carbon nanotubes into a graphite mold. Cut graphite paper to match the size of the graphite mold and cover the mixed powder in the graphite mold. Lifting platform 2 lowers the reaction chamber to an open space, stacks multiple graphite molds in the center of the reaction chamber, and then raises the reaction chamber into the box-type furnace body 1. S2: Start the box-type furnace body 1, adjust the flow rate of nitrogen gas, and heat the temperature of the reaction chamber to a set temperature of 1450-1550°C at a heating rate of 3-10°C / min. Nitrogen gas is introduced into the reaction chamber through the air inlet 7 and the air inlet 5 to react with the mixed powder in the gas phase for 3-6 hours, and then discharged through the air outlet and the air outlet 6; the flow rate of nitrogen gas introduced into each of the air inlet and the air inlet is 0.5-2 L / min; S3: After the reaction is completed, the reaction chamber is cooled to room temperature, and the lifting platform 2 drives the reaction chamber down to the open space, takes out the graphite paper, collects the product on the graphite paper, and obtains a silicon nitride nanowire flexible ceramic film.

[0042] Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiments are only used to illustrate the present invention and are not used in limiting the scope of the present invention.In addition, should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms fall equally within the scope limited by the appended claims of the application.

[0043] The following examples were prepared using conventional instruments and equipment in the art. Experimental methods in the following examples, where specific conditions are not specified, were generally performed under conventional conditions or according to the conditions recommended by the manufacturer. The various raw materials used in the following examples, unless otherwise specified, were conventional commercially available products, with specifications conventional in the art. In the present specification and the following examples, unless otherwise specified, "%" indicates percentage by weight, "part" indicates parts by weight, and "ratio" indicates weight ratio.

[0044] Example 1 S1: 17 g of a mixed powder of silicon dioxide and carbon nanotubes in a mass ratio of 5:1 is placed into a graphite mold. Graphite paper is cut to match the size of the graphite mold and covered over the mixed powder in the graphite mold. Lifting platform 2 lowers the reaction chamber to an open space, stacks multiple graphite molds in the center of the reaction chamber, and then raises the reaction chamber into the box-type furnace body 1. S2: Start the box furnace body 1, adjust the flow rate of nitrogen gas, and heat the temperature of the reaction chamber to a set temperature of 1480°C at a heating rate of 3°C / min. Nitrogen gas is introduced into the reaction chamber through the air inlet 7 and the air inlet 5 to react with the mixed powder in the gas phase for 3 hours, and then discharged through the air outlet and the air outlet 6; the flow rate of nitrogen gas introduced into each of the air inlet and the air inlet is 0.8 L / min; S3: After the reaction is completed, the reaction chamber is cooled to room temperature, and the lifting platform 2 drives the reaction chamber down to the open space, takes out the graphite paper, collects the product on the graphite paper, and obtains a silicon nitride nanowire flexible ceramic film.

[0045] like Figure 5 and Figure 6As shown, in Example 1, a uniform silicon nitride nanowire flexible ceramic film with a size of 220*180 mm was prepared. A single silicon nitride nanowire was in a linear shape with a diameter of 200-500 nm and a length of several microns.

[0046] Example 2 S1: 17 g of a mixed powder of silicon dioxide and carbon nanotubes in a mass ratio of 5:2 is placed into a graphite mold. Graphite paper is cut to match the size of the graphite mold and covered over the mixed powder in the graphite mold. Lifting platform 2 lowers the reaction chamber to an open space, and multiple graphite molds are stacked in the center of the reaction chamber. The reaction chamber is then raised into the box-type furnace body 1. S2: Start the box furnace body 1, adjust the flow rate of nitrogen gas, and heat the temperature of the reaction chamber to a set temperature of 1450°C at a heating rate of 4°C / min. Nitrogen gas is introduced into the reaction chamber through the air inlet 7 and the air inlet 5 to react with the mixed powder in the gas phase for 4 hours, and then discharged through the air outlet and the air outlet 6; the flow rate of nitrogen gas introduced into each of the air inlet and the air inlet is 1 L / min; S3: After the reaction is completed, the reaction chamber is cooled to room temperature, and the lifting platform 2 drives the reaction chamber down to the open space, takes out the graphite paper, collects the product on the graphite paper, and obtains a silicon nitride nanowire flexible ceramic film.

[0047] See also Figure 7 In this embodiment 2, a uniform silicon nitride nanowire flexible ceramic film with a size of 200*180 mm was prepared.

[0048] Example 3 S1: 17 g of a mixed powder consisting of silicon dioxide and carbon nanotubes in a mass ratio of 5:3 is placed into a graphite mold. Graphite paper is cut to match the size of the graphite mold and covered over the mixed powder in the graphite mold. Lifting platform 2 lowers the reaction chamber to an open space, stacks multiple graphite molds in the center of the reaction chamber, and then raises the reaction chamber into the box-type furnace body 1. S2: Start the box furnace body 1, adjust the flow rate of nitrogen gas, and heat the temperature of the reaction chamber to a set temperature of 1550°C at a heating rate of 8°C / min. Nitrogen gas is introduced into the reaction chamber through the air inlet 7 and the air inlet 5 to react with the mixed powder in the gas phase for 3 hours, and then discharged through the air outlet and the air outlet 6; the flow rate of nitrogen gas introduced into each of the air inlet and the air inlet is 0.5 L / min; S3: After the reaction is completed, the reaction chamber is cooled to room temperature, and the lifting platform 2 drives the reaction chamber down to the open space, takes out the graphite paper, collects the product on the graphite paper, and obtains a silicon nitride nanowire flexible ceramic film.

[0049] See also Figure 8In this embodiment 3, a uniform silicon nitride nanowire flexible ceramic film with a size of 225*180 mm was prepared.

[0050] Example 4 S1: 17 g of a mixed powder of silicon dioxide and carbon nanotubes in a mass ratio of 4:1 is placed into a graphite mold. Graphite paper is cut to match the size of the graphite mold and covered over the mixed powder in the graphite mold. Lifting platform 2 lowers the reaction chamber to an open space, and multiple graphite molds are stacked in the center of the reaction chamber. The reaction chamber is then raised into the box-type furnace body 1. S2: Start the box furnace body 1, adjust the flow rate of nitrogen gas, and heat the temperature of the reaction chamber to a set temperature of 1500°C at a heating rate of 5°C / min. Nitrogen gas is introduced into the reaction chamber through the air inlet 7 and the air inlet 5 to react with the mixed powder in the gas phase for 3.5 hours, and then discharged through the air outlet and the air outlet 6; the flow rate of nitrogen gas introduced into each of the air inlet and the air inlet is 2 L / min; S3: After the reaction is completed, the reaction chamber is cooled to room temperature, and the lifting platform 2 drives the reaction chamber down to the open space, takes out the graphite paper, collects the product on the graphite paper, and obtains a silicon nitride nanowire flexible ceramic film.

[0051] See also Figure 9 In this embodiment 4, a uniform silicon nitride nanowire flexible ceramic film with a size of 185*150 mm was prepared.

[0052] Example 5 S1: 17 g of a mixed powder of silicon dioxide and carbon nanotubes in a mass ratio of 4:3 is placed into a graphite mold. Graphite paper is cut to match the size of the graphite mold and covered over the mixed powder in the graphite mold. Lifting platform 2 lowers the reaction chamber to an open space, and multiple graphite molds are stacked in the center of the reaction chamber. The reaction chamber is then raised into the box-type furnace body 1. S2: Start the box furnace body 1, adjust the flow rate of nitrogen gas, and heat the temperature of the reaction chamber to a set temperature of 1460°C at a heating rate of 7°C / min. Nitrogen gas is introduced into the reaction chamber through the air inlet 7 and the air inlet 5 to react with the mixed powder in the gas phase for 4 hours, and then discharged through the air outlet and the air outlet 6; the flow rate of nitrogen gas introduced into each of the air inlet and the air inlet is 1.5 L / min; S3: After the reaction is completed, the reaction chamber is cooled to room temperature, and the lifting platform 2 drives the reaction chamber down to the open space, takes out the graphite paper, collects the product on the graphite paper, and obtains a silicon nitride nanowire flexible ceramic film.

[0053] See also Figure 10 In this embodiment 5, a uniform silicon nitride nanowire flexible ceramic film with a size of 210*160 mm was prepared.

[0054] Example 6 S1: 17 g of a mixed powder consisting of silicon dioxide and carbon nanotubes in a mass ratio of 6:1 is placed into a graphite mold. Graphite paper is cut to match the size of the graphite mold and covered over the mixed powder in the graphite mold. Lifting platform 2 lowers the reaction chamber to an open space, stacks multiple graphite molds in the center of the reaction chamber, and then raises the reaction chamber into the box-type furnace body 1. S2: Start the box furnace body 1, adjust the flow rate of nitrogen gas, and heat the temperature of the reaction chamber to a set temperature of 1465°C at a heating rate of 9°C / min. Nitrogen gas is introduced into the reaction chamber through the air inlet 7 and the air inlet 5 to react with the mixed powder in the gas phase for 6 hours, and then discharged through the air outlet and the air outlet 6; the flow rate of nitrogen gas introduced into each of the air inlet and the air inlet is 1.2 L / min; S3: After the reaction is completed, the reaction chamber is cooled to room temperature, and the lifting platform 2 drives the reaction chamber down to the open space, takes out the graphite paper, collects the product on the graphite paper, and obtains a silicon nitride nanowire flexible ceramic film.

[0055] See also Figure 11 In this embodiment 6, a uniform silicon nitride nanowire flexible ceramic film with a size of 210*180 mm was prepared.

[0056] Example 7 S1: 17 g of a mixed powder of silicon dioxide and carbon nanotubes in a mass ratio of 3:1 is placed in a graphite mold. Graphite paper is cut to match the size of the graphite mold and covered on the mixed powder in the graphite mold. Lifting platform 2 drives the reaction chamber down to the open space, multiple graphite molds are stacked in the center of the reaction chamber, and then the reaction chamber is raised to the box-type furnace body 1. S2: Start the box furnace body 1, adjust the flow rate of nitrogen gas, and heat the temperature of the reaction chamber to a set temperature of 1530°C at a heating rate of 10°C / min. Nitrogen gas is introduced into the reaction chamber through the air inlet 7 and the air inlet 5 to react with the mixed powder in the gas phase for 5 hours, and then discharged through the air outlet and the air outlet 6; the flow rate of nitrogen gas introduced into each of the air inlet and the air inlet is 1.5 L / min; S3: After the reaction is completed, the reaction chamber is cooled to room temperature, and the lifting platform 2 drives the reaction chamber down to the open space, takes out the graphite paper, collects the product on the graphite paper, and obtains a silicon nitride nanowire flexible ceramic film.

[0057] See also Figure 12 In this embodiment 7, a uniform silicon nitride nanowire flexible ceramic film with a size of 200*165 mm was prepared.

[0058] The above content is only for explaining the technical idea of the present invention and cannot be used to limit the protection scope of the present invention. Any changes made on the basis of the technical solution in accordance with the technical idea proposed by the present invention shall fall within the protection scope of the claims of the present invention.

Claims

1. A device for batch production of silicon nitride nanowire flexible ceramic films, characterized in that: The invention comprises a box-type furnace body (1), wherein an open space is provided at the bottom of the box-type furnace body (1), and a lifting platform (2) is installed inside the open space; a detachable reaction chamber composed of a plurality of brick bodies is supported above the lifting platform (2), and a graphite mold is placed inside the reaction chamber; the inner wall of the box-type furnace body (1) and the outer wall of the reaction chamber are arranged close to each other, and a plurality of air inlets (7) and air inlets (5) arranged in an array are respectively provided on the side walls on the same side of the box-type furnace body, and the air inlets (7) and the air inlets (5) correspond to each other, and a plurality of air outlets (6) and the air outlet are respectively provided on the side walls on the opposite side, and the air outlets (6) and the air outlet are aligned.

2. The device for mass production of silicon nitride nanowire flexible ceramic films according to claim 1, characterized in that: The reaction chamber is composed of a plurality of bricks joined in a mortise and tenon manner; the graphite mold comprises a bearing plate surface and four groups of limit blocks arranged at the four corners of the bearing plate surface.

3. The device for mass production of silicon nitride nanowire flexible ceramic films according to claim 1, characterized in that: A heating mechanism is provided on the inner wall of the reaction chamber, and a control panel (3) is provided outside the box-type furnace body (1). The control panel (3) is electrically connected to the heating mechanism and is used to control the temperature inside the reaction chamber.

4. The device for mass production of silicon nitride nanowire flexible ceramic films according to claim 1, characterized in that: The air inlet hole (7) and the air inlet port (5) are connected to a plurality of air inlet pipes, the air inlet pipes being arranged on an air pipe rack, the inlets of the air inlet pipes being connected to an air source; the air inlet pipes are connected to an air pump, and a flow meter is arranged on the air inlet pipes, and the flow meter is used to control the air inlet flow rate.

5. The device for mass production of silicon nitride nanowire flexible ceramic films according to claim 1, characterized in that: The open space is a space formed by a cubic frame; the lifting platform (2) is an electric push rod lifting platform consisting of a table top and a lifting rod located in the middle of the table top.

6. The device for mass production of silicon nitride nanowire flexible ceramic films according to claim 1, characterized in that: The air outlet (6) is connected to a plurality of tail gas bottles; the apertures of the air inlet (7) and the air inlet (5) are equal, the apertures of the air outlet (6) and the air outlet are equal, and the apertures of the air inlet (7) and the air inlet (5) are smaller than the apertures of the air outlet (6) and the air outlet.

7. A method for batch production of silicon nitride nanowire flexible ceramic films, characterized in that: The device for mass production of silicon nitride nanowire flexible ceramic films according to any one of claims 1 to 6 is characterized in that it comprises the following steps: A mixed powder of silicon dioxide and carbon nanotubes is placed in a graphite mold, and graphite paper is cut to match the size of the graphite mold and covered on the mixed powder in the graphite mold; a lifting platform (2) drives the reaction chamber down to an open space, and multiple graphite molds are stacked in the reaction chamber, and then the reaction chamber is driven up to the box-type furnace body (1); The box-type furnace body (1) is started, the flow rate of the nitrogen gas introduced is adjusted, the temperature of the reaction chamber is raised to the set temperature, the nitrogen gas is introduced into the reaction chamber through the air inlet (7) and the air inlet (5) to react with the mixed powder in the gas phase, and then discharged through the air outlet and the air outlet (6); After the reaction is completed, the reaction chamber is cooled to room temperature, and the lifting platform (2) drives the reaction chamber down to an open space, takes out the graphite paper, collects the product on the graphite paper, and obtains a silicon nitride nanowire flexible ceramic film.

8. The method for mass production of silicon nitride nanowire flexible ceramic films according to claim 7, characterized in that: The set temperature is 1450-1550° C.; the gas phase reaction time is 3-6 hours.

9. The method for mass production of silicon nitride nanowire flexible ceramic films according to claim 7, characterized in that: The nitrogen flow rate introduced into each of the air inlet holes (7) and the air inlet (5) is 0.5-2 L / min.

10. The method for mass production of silicon nitride nanowire flexible ceramic films according to claim 7, characterized in that: The temperature of the temperature-elevated reaction chamber is increased at a rate of 3-10° C. / min.

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