Apparatus and method for synthesizing boron nitride nanotubes

Abstract

According to an embodiment of the present invention, disclosed is an apparatus for synthesizing boron nitride nanotubes, the apparatus comprising: a storage unit which accommodates precursor units arranged in a plurality of rows, each precursor unit including a plurality of precursors; a reaction unit which receives the precursor units accommodated in the storage unit and synthesizes nanomaterials from the precursors; and a supply unit which is connected to the storage unit and the reaction unit, receives the precursor units row by row from the storage unit, and supplies the precursor units to the reaction unit, wherein the reaction unit includes a plurality of tubular chambers into which the precursors in the precursor units are simultaneously introduced respectively, and the reaction unit includes at least one heater and a first zone, a second zone, and a third zone that have different average temperatures, the average temperature of the third zone being higher than the average temperatures of the first zone and the second zone.

Description

Boron nitride nanotube synthesis device and synthesis method

[0001] The present invention relates to a boron nitride nanotube synthesis device and synthesis method.

[0002] Nanoscale materials have attracted much attention in various industries, including the electronics industry, due to their numerous excellent properties. However, practical industrial application has been difficult due to limitations in the process for mass-producing high-quality nanomaterials.

[0003] Among various nanoscale materials, boron nitride nanotubes (BNNTs) in particular possess similar mechanical and thermal conductivity properties to the more commonly known carbon nanotubes (CNTs), while also exhibiting superior electrical insulation, heat resistance, and chemical stability. Furthermore, the boron that composes BNNTs has a thermal neutron absorption capacity that is approximately 200,000 times higher than that of the carbon that composes CNTs, making them useful as neutron shielding materials.

[0004] However, due to the difficulty of synthesizing BNNTs at high temperatures exceeding 1,000°C, mass production is currently difficult worldwide. This situation is not limited to BNNTs; the development of high-quality mass production technology is also necessary for other nanomaterials.

[0005] Embodiments of the present invention provide a device capable of mass-producing and efficiently synthesizing boron nitride nanotubes.

[0006] However, the technical problems to be solved by the present invention are not limited to the problems described above, and other problems not mentioned can be clearly understood by those skilled in the art from the description of the invention described below.

[0007] One embodiment of the present invention discloses a boron nitride nanotube synthesis device, comprising: a receiving unit that receives precursor units each including a plurality of precursors and forming a plurality of rows; a reaction unit that receives the precursor units received in the receiving unit and synthesizes nanomaterials from the precursors; and a supply unit that is connected to the receiving unit and the reaction unit and receives the precursor units one row at a time from the receiving unit and supplies them to the reaction unit; wherein the reaction unit includes a plurality of tubular chambers into which the precursors of the precursor units are simultaneously introduced, and the reaction unit includes at least one heater and a first region, a second region, and a third region having different average temperatures, and wherein the average temperature of the third region is higher than the average temperatures of the first region and the second region.

[0008] According to embodiments of the present invention, it is possible to synthesize boron nitride nanotubes in large quantities, and the efficiency of the manufacturing process can be improved.

[0009] Additionally, the manufacturing yield can be improved by directly injecting the reaction gas required for synthesis into the chamber.

[0010] However, the effects that can be obtained through the present invention are not limited to the effects described above, and other technical effects not mentioned can be clearly understood by those skilled in the art from the description of the invention described below.

[0011] The following drawings attached to this specification illustrate preferred embodiments of the present invention, and together with the detailed description of the invention described below, serve to further understand the technical idea of ​​the present invention, and therefore, the present invention should not be interpreted as being limited to matters described in such drawings.

[0012] FIG. 1 is a schematic diagram illustrating an example of a boron nitride nanotube synthesis device according to one embodiment of the present invention.

[0013] FIG. 2 is a flowchart schematically illustrating a method for synthesizing boron nitride nanotubes according to one embodiment of the present invention.

[0014] FIG. 3 is a perspective view schematically illustrating an example of a precursor for synthesizing nanomaterials according to one embodiment of the present invention.

[0015] Fig. 4 is a cross-sectional view schematically illustrating an example of the AA' cross-section of Fig. 3.

[0016] FIG. 5 is a schematic plan view illustrating an example of a supply section and a reaction section of the boron nitride nanotube synthesis device of FIG. 1.

[0017] Fig. 6 is a schematic plan view of an example of a storage unit of the boron nitride nanotube synthesis device of Fig. 1.

[0018] Fig. 7 is a schematic plan view illustrating an example of a pusher of a supply section of the boron nitride nanotube synthesis device of Fig. 1.

[0019] Fig. 8 is a schematic plan view illustrating an example of a reaction section of the boron nitride nanotube synthesis device of Fig. 1.

[0020] Fig. 9 is a perspective view schematically illustrating an example of a chamber and piping of the reaction unit of Fig. 8.

[0021] Fig. 10 is a perspective view schematically illustrating another example of the chamber and piping of the reaction unit of Fig. 8.

[0022] Fig. 11 is a perspective view schematically illustrating another example of the chamber and piping of the reaction unit of Fig. 8.

[0023] Fig. 12 is a perspective view schematically illustrating another example of the chamber and piping of the reaction unit of Fig. 8.

[0024] One embodiment of the present invention discloses a boron nitride nanotube synthesis device, comprising: a receiving unit that receives precursor units each including a plurality of precursors and forming a plurality of rows; a reaction unit that receives the precursor units received in the receiving unit and synthesizes nanomaterials from the precursors; and a supply unit that is connected to the receiving unit and the reaction unit and receives the precursor units one row at a time from the receiving unit and supplies them to the reaction unit; wherein the reaction unit includes a plurality of tubular chambers into which the precursors of the precursor units are simultaneously introduced, and the reaction unit includes at least one heater and a first region, a second region, and a third region having different average temperatures, and wherein the average temperature of the third region is higher than the average temperatures of the first region and the second region.

[0025] In this embodiment, the precursor may be a precursor for synthesizing boron nitride nanotubes.

[0026] In the present embodiment, the supply unit may include at least one pusher that introduces the precursor units into the reaction unit.

[0027] In this embodiment, the pusher can simultaneously push the precursors of the precursor units of the one row.

[0028] In this embodiment, the storage unit can be slidable up and down.

[0029] In this embodiment, the outer surface of the storage unit may include a guide unit that guides movement of the storage unit.

[0030] In this embodiment, each of the chambers may be connected to two or more pipes supplying reaction gas.

[0031] In the present embodiment, the reaction section may further include a fourth region and a fifth region having different average temperatures and having a lower average temperature than the third region.

[0032] Another embodiment of the present invention discloses a method for synthesizing boron nitride nanotubes, comprising: a step of delivering precursor units each including a plurality of precursors and forming a plurality of rows to a supply unit; a step of simultaneously introducing the precursors of a single row of precursor units into a reaction unit by a pusher; a step of synthesizing nanomaterials by reacting the precursor units with a reaction gas introduced into the reaction unit in the reaction unit; and a step of discharging the synthesized nanomaterials from the reaction unit to a discharge unit; wherein the reaction unit includes a plurality of tubular chambers into which the precursors of the precursor units are each simultaneously introduced, and the reaction unit includes at least one heater and a first region, a second region, and a third region having different average temperatures, wherein the average temperature of the third region is higher than the average temperature of the second region.

[0033] In this embodiment, the rate of change in temperature over time of the reaction section may be 4°C to 9°C.

[0034] In this embodiment, each of the chambers may be connected to two or more pipes supplying reaction gas.

[0035] In the present embodiment, in the step of delivering to the supply unit, the receiving unit can slide in the direction of the supply unit to deliver the precursor units to the supply unit.

[0036] In this embodiment, when all of the precursor units stored in the storage unit are supplied to the supply unit, the storage unit can slide in the opposite direction to the supply unit.

[0037] In this embodiment, the nanomaterial can be synthesized in the third region.

[0038] In the present embodiment, the reaction section may further include a fourth region and a fifth region having different average temperatures and having a lower average temperature than the third region.

[0039] Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the attached drawings. Prior to this, terms or words used in this specification and claims should not be interpreted as limited to their typical or dictionary meanings, and should be interpreted with meanings and concepts that conform to the technical spirit of the present invention based on the principle that the inventor can appropriately define the concept of a term to best explain his or her own invention. Therefore, the embodiments described in this specification and the configurations illustrated in the drawings are only some of the most preferred embodiments of the present invention and do not represent all of the technical spirit of the present invention. Therefore, it should be understood that various equivalents and modified examples may exist as substitutes for them at the time of filing this application.

[0040] Additionally, when used herein, the terms "comprise", "include" and / or "comprising", "including" specify the presence of stated features, numbers, steps, operations, elements, elements and / or groups thereof, but do not preclude the presence or addition of one or more other features, numbers, operations, elements, elements and / or groups thereof.

[0041] Additionally, to facilitate understanding of the invention, the attached drawings are not drawn to scale and some components may be exaggerated in size. Furthermore, identical components may be assigned the same reference numbers in different embodiments.

[0042] Although terms like "first" and "second" are used to describe various components, these components are not limited by these terms. These terms are used merely to distinguish one component from another, and unless otherwise specified, a "first" component may also be a "second" component.

[0043] Throughout the specification, unless otherwise specifically stated, each element may be singular or plural.

[0044] Any configuration being placed "on (or under)" or "above (or below)" a component may mean not only that any configuration is placed in contact with the upper surface (or lower surface) of said component, but also that other configurations may intervene between said component and any configuration placed on (or below) said component.

[0045] Additionally, when it is described that a component is "connected," "coupled," or "connected" to another component, it should be understood that the components may be directly connected or connected to one another, but that other components may also be "interposed" between the components, or that each component may be "connected," "coupled," or "connected" through another component. Furthermore, when it is said that a part is electrically coupled to another part, this includes not only cases where they are directly connected, but also cases where they are connected with another element in between.

[0046] FIG. 1 is a schematic diagram illustrating an example of a boron nitride nanotube synthesis device according to an embodiment of the present invention, FIG. 2 is a flowchart schematically illustrating a boron nitride nanotube synthesis method according to an embodiment of the present invention, FIG. 3 is a perspective view schematically illustrating an example of a precursor for nanomaterial synthesis according to an embodiment of the present invention, FIG. 4 is a cross-sectional view schematically illustrating an example of a section taken along line AA' of FIG. 3, FIG. 5 is a plan view schematically illustrating an example of a supply unit and a reaction unit of the boron nitride nanotube synthesis device of FIG. 1, FIG. 6 is a plan view schematically illustrating an example of a receiving unit of the boron nitride nanotube synthesis device of FIG. 1, FIG. 7 is a plan view schematically illustrating an example of a pusher of the supply unit of the boron nitride nanotube synthesis device of FIG. 1, FIG. 8 is a plan view schematically illustrating an example of a reaction unit of the boron nitride nanotube synthesis device of FIG. 1, and FIG. 9 is a plan view schematically illustrating an example of a chamber and a pipe of the reaction unit of FIG. 8. It's a perspective view.

[0047] Referring to FIGS. 1 to 9, a boron nitride nanotube synthesis device (1000) according to one embodiment of the present invention may include a receiving unit (100) that receives precursor units (20) each including a plurality of precursors (10) and forming a plurality of rows, a reaction unit (300) that receives the precursor units (20) received in the receiving unit (100) and synthesizes nanomaterials in the precursor units (20), a supply unit (200) that is connected to the receiving unit (100) and the reaction unit (300) and receives the precursor units (20) one row at a time from the receiving unit (100) and supplies them to the reaction unit (300), a discharge unit (400) that discharges nanomaterials synthesized in the reaction unit (300), and a storage unit (500) that is connected to the discharge unit (400) and stores the synthesized nanomaterials.

[0048] In addition, a method (S100) for synthesizing boron nitride nanotubes according to one embodiment of the present invention may include a step (S110) of transferring precursor units (20) each including a plurality of precursors (10) to form a plurality of rows from a receiving unit (100) to a supply unit (200), a step (S120) of simultaneously introducing the precursors (10) of one row of precursor units (20) into a reaction unit (300) by a pusher (210), a step (S130) of reacting the precursor units (20) and the reaction gas introduced into the reaction unit (300) in the reaction unit (300) to synthesize a nanomaterial, and a step (S140) of discharging the synthesized nanomaterial from the reaction unit (300) to a discharge unit (400).

[0049] Referring to FIG. 3, a precursor (10) for synthesizing nanomaterials according to one embodiment of the present invention may include at least one receiving portion formed along the longitudinal direction (x) of the precursor (10). The receiving portion may include, for example, receiving grooves (12, 12'). However, the present invention is not limited thereto, and the receiving portion may, for example, include at least one flat receiving surface on the upper and lower surfaces of the precursor (10) so that the precursor (10) can be stored while being stacked in layers. The receiving surface may be formed as a flat, continuous surface along the longitudinal direction of the precursor (10).

[0050] As another example, the receiving portion may include a plurality of through holes extending from the outside to the inside of the precursor (10). The plurality of through holes may be formed radially with respect to an imaginary line passing through the central axis of the precursor (10), and the plurality of through holes may be provided spaced apart from each other along the longitudinal direction of the precursor (10). For example, the receiving groove (12, 12') may be in communication with at least one of the plurality of through holes.

[0051] The storage grooves (12, 12') may be formed along the longitudinal direction (x) of the precursor (10) and in a direction from the outer side (or outer circumference) of the precursor toward the inner side. In addition, the storage grooves (12, 12') may be provided symmetrically on the upper and lower surfaces of the precursor (10), for example, with respect to a plane passing through the central axis of the precursor (10).

[0052] The precursor (10) may be, for example, a precursor for synthesizing boron nitride nanotubes (BNNTs). Boron nitride nanotubes are hexagonal nanotubes in which nitrogen (N) and boron (B) are alternately arranged, and have excellent thermal conductivity properties, but also have a wide band gap, so they have electrically insulating properties similar to ceramics. Therefore, although boron nitride nanotubes are electrically insulating, they can be applied as high thermal conductivity composites.

[0053] In addition, boron nitride nanotubes have excellent mechanical properties, chemical resistance and oxidation resistance, absorb thermal neutrons, and are known to be harmless to the human body, so they can be applied to various industrial fields such as electronics, energy, space, nuclear power, and bio-medical.

[0054] Meanwhile, the precursor (10) may have a cylindrical shape. At this time, the “cylindrical shape” includes not only a basic cylindrical shape but also a shape that is modified based on a cylindrical shape. Since the precursor (10) has a cylindrical shape, it can be easily introduced into the chamber of the boron nitride nanotube synthesis device (1000) described below and can be easily stored in the storage unit (100). Through this, there is an advantage of improving the efficiency of the nanomaterial synthesis process in the boron nitride nanotube synthesis device (1000) and reducing the difficulty of the process.

[0055] A method for manufacturing a precursor (10) may include a step of preparing a first powder including raw material powder and a catalyst, a step of nano-forming the first powder to obtain a second powder, a step of manufacturing a dispersion including the second powder, a step of molding the dispersion to obtain a columnar precursor (10) for nano-material synthesis, and a step of creating micropores (P) in the precursor (10) to obtain a porous precursor (10) for nano-material synthesis.

[0056] The above raw material powder may be, for example, powdered boron. Specifically, the boron may be amorphous and / or crystalline boron. Since amorphous boron has low hardness, it not only efficiently contributes to the nano-ization of catalyst metal and / or metal oxide particles that are mixed and added during the nano-ization step, specifically, the nano-ization process of the boron powder using air vortex, but also allows the boron powder to be coated or embedded on the surface of the catalyst metal and / or metal oxide to obtain efficient seed precursor nanoparticles.

[0057] The catalyst may be provided in powder form. The catalyst may be more effective with amorphous boron. This is because, when amorphous boron is used, a large amount of boron nanopowder can be produced in a very short period of time through a nano-forming process using an air jet and / or its vortex. The catalyst is not particularly limited, and for example, the catalyst may include Fe, Mg, Ni, Cr, Co, Zr, Mo, W, and / or Ti, and oxides thereof.

[0058] The above catalyst is mixed with raw material powder particles during the nano-forming process of raw material powder to form precursor nanoparticles. These precursor nanoparticles can serve as seeds in the production of nanomaterials and contribute to the synthesis of nanomaterials by reacting with gases. For example, boron precursor nanoparticles can contribute to the synthesis of boron nitride nanotubes by reacting with nitrogen.

[0059] The first powder can be nanosized by injecting the first powder into a grinding zone formed by air. For example, the first powder can be nanosized through air jet milling. At this time, the process conditions of the air jet milling may be as follows: the feed rate of the first powder may be 2 g / min or more and 10 g / min or less, the feed pressure may be 80 psi or more and 120 psi or less, and the grinding pressure may be 60 psi or more and 100 psi or less. Through the air jet milling process under the above conditions, the first powder can be effectively nanosized. Through this, a catalyst can be embedded in the boron powder, which can act as a major factor in the subsequent nanotube growth.

[0060] The above dispersion may include the second powder, binder powder, and a foaming agent. At this time, the weight ratio of the second powder, binder powder, and foaming agent may be 1:1 to 4:0.1 to 0.2. At this time, as the binder powder and foaming agent, those used in the art may be used without limitation.

[0061] The step of molding a dispersion containing the second powder to obtain a precursor (10) for synthesizing a columnar nanomaterial may include a step of injecting the dispersion into a columnar mold and heating the mold. The temperature at which the mold is heated may be 150°C or more and 250°C or less, and the time for heating the mold may be 0.5 hours or more and 8 hours or less.

[0062] By heat-treating the mold under the temperature and time conditions of the aforementioned range, a precursor for synthesizing a columnar nanomaterial can be easily obtained. At this time, the step of obtaining the precursor for synthesizing a columnar nanomaterial and the step of obtaining the porous precursor for synthesizing a nanomaterial can be performed simultaneously. For example, a precursor (10) for synthesizing a nanomaterial having a columnar shape and a porous structure can be obtained through a process of placing a dispersion liquid in a cylindrical mold and performing a heat treatment.

[0063] Meanwhile, the precursor (10) for nanomaterial synthesis has a lower heat capacity than the reaction module, so it can be introduced at a high speed into the chamber (330) of the boron nitride nanotube synthesis device (1000) described later, thereby effectively improving the efficiency of the boron nitride nanotube synthesis process.

[0064] In addition, the precursor (10) for synthesizing nanomaterials can be introduced into the chamber (330) without a reaction module, making maintenance easy and reducing the production cost of synthesizing boron nitride nanotubes. In addition, since the precursor (10) for synthesizing nanomaterials is lightweight, the possibility of damage to the nanotube synthesis device (1000) due to thermal shock to the components of the nanotube synthesis device (1000) is low, thereby improving the stability of the nanomaterial synthesis system.

[0065] Meanwhile, the storage unit (100) and the supply unit (200) of the boron nitride nanotube synthesis device (1000) may be provided with fastening units corresponding to the storage grooves (12, 12'). Accordingly, the precursor (10) can be stably stored in the storage unit (100), making stacking and storage of the precursor (10) easier.

[0066] In addition, the precursor (10) fed from the storage unit (100) to the supply unit (200) can be arranged to align with the position of the pusher to be described later in the supply unit (200), so that the boron nitride nanotube synthesis device (1000) can be automated, and the precursor (10) can be easily fed from the supply unit (200) to the reaction unit (300).

[0067] In the reaction section (300), a fastening member or guide member corresponding to a receiving groove (12, 12') may be arranged in the chamber where the precursor (10) moves and the nanomaterial is synthesized. As a result, the precursor (10) can move without falling out of the chamber (330).

[0068] Conventional precursors do not have a separate storage compartment formed, so the precursor is placed in a reaction module and then injected into the reaction unit, which has the problem of low process efficiency. On the other hand, the precursor (10) according to one embodiment of the present invention has a storage compartment formed therein, so it can be directly injected into a boron nitride nanotube synthesis device (1000) without a separate reaction module, effectively improving process efficiency and enabling the synthesis of nanomaterials in large quantities.

[0069] Referring to Fig. 4, the ratio of the diameter of the precursor (10) to the diameter (d2') of the receiving groove (12, 12') may be 1:0.0001 to 1:0.3. When the length ratio of the diameter of the precursor (10) to the diameter (d2') of the receiving groove (12, 12') is within the aforementioned range, the precursor (10) can be stably received in the receiving portion (100) through the receiving groove (12, 12'), and the mechanical properties of the precursor (10), such as strength and durability, can be effectively suppressed from deteriorating.

[0070] In addition, the ratio of the diameter of the precursor (10) and the length of the precursor (10) may be 1:3 or more and 1:6. When the ratio of the diameter and length of the precursor (10) is within the above-mentioned range, the reaction gas can be effectively supplied to the precursor (10) within the chamber (330) of the boron nitride nanotube synthesis device (1000), thereby further increasing the synthesis efficiency of the nanomaterial. In addition, by adjusting the ratio of the diameter and length of the precursor (10) within the above-mentioned range, the precursor (10) can be effectively stored in the storage unit (100) and easily introduced into the chamber (330).

[0071] Meanwhile, the diameter (d2') of the storage groove (12, 12') may refer to the shortest length among the lengths passing through the central axis of the storage groove (12, 12'), and the diameter of the precursor (10) may refer to the longest length among the lengths passing through the central axis in the cross section of the precursor (e.g., a cylinder). In addition, the diameter of the precursor may be variously changed according to the diameter of the chamber of the boron nitride nanotube synthesis device (1000) described later.

[0072] Meanwhile, the precursor (10) may have a porous structure. For example, the precursor (10) may have a porous structure including a plurality of micropores (P). In this case, for convenience of explanation, the micropores (P) are enlarged and illustrated in FIG. 4. In addition, although FIG. 4 discloses that the precursor (10) includes a plurality of micropores (P) inside, a plurality of micropores (P) may also be formed on the outer surface of the precursor (10). When the precursor (10) has a porous structure, the contact area with the reaction gas described later is further increased, so that the efficiency of nanomaterial synthesis can be further improved.

[0073] Referring to FIG. 6 together with FIG. 1, the storage unit (100) may include a storage gate (110) that is connected to the supply unit (200) and can be opened and closed, a partition wall (120) that partitions the precursor (10) along the height direction (z) of the storage unit, a placement unit (130) in which the precursor (10) is placed, and a guide unit (140) that guides the movement of the storage unit (100).

[0074] The precursor (10) can be stored in a space partitioned by a partition wall (120) and a mounting portion (130). Accordingly, the precursor (10) can be isolated from other precursors (10) adjacent to it. As a result, the precursor (10) can be independently introduced into a chamber described below.

[0075] The fixing member (130) may be provided with a fastening member corresponding to the storage groove (12, 12') formed in the precursor (10). Accordingly, the precursor (10) can be stably stored in the storage member (100), making stacking and storage of the precursor (10) easier.

[0076] In Fig. 6, the fixing portion (130) is shown as having a fastening portion corresponding to the receiving groove (12, 12') formed in the precursor (10), but this is not limited thereto, and as another example, the receiving portion (100) may include a separate jig corresponding to the shape of the precursor (10), and the precursor (10) may be accommodated in each of the jigs.

[0077] As another example, when the storage portion includes a storage surface as described above, the mounting portion (130) may be omitted, and the precursors (10) may be stored by being stacked in layers along the flat storage surface.

[0078] Meanwhile, precursor units (20) each including a plurality of precursors (10) to form a plurality of rows can be stored in each row of the storage unit (100). The precursor unit (20) can include at least one precursor (10). For example, the precursor unit (20) can include four precursors (10) as shown in FIG. 6, but is not limited thereto, and the number of precursors (10) included in the precursor unit (20) can be changed as needed.

[0079] The storage gate (110) connecting the storage unit (100) and the supply unit (200) may be opened and closed. As the storage gate (110) is opened, the precursor units (20) stored in each row of the storage unit (100) may be transferred to the supply unit (200). At this time, the storage gate (110) may be driven so that one precursor unit (20) is supplied from the storage unit (100) to the supply unit (200).

[0080] In the step (S110) of transferring a plurality of precursor units (20) from the storage unit (100) to the supply unit (200), when the storage gate (110) is opened, the storage unit (100) can slide in the direction (z) of the supply unit (200) to supply the precursor units (20) one row at a time to the supply unit (200). That is, the precursor units (20) can be supplied in a bullet-like manner from the storage unit (100) to the supply unit (200).

[0081] When all of the precursor units (20) stored in the storage unit (100) are supplied to the supply unit (200), the storage unit (100) can be restored by sliding in the opposite direction (-z) to the supply unit. Once the storage unit (100) is restored, new precursor units (20) can be stored in the storage unit (100) again, and the above-described process can be repeated.

[0082] As in one embodiment of the present invention, by continuously supplying precursor units (20) including at least one precursor (10) to the supply unit (200), the storage unit (100) enables synthesis of nanomaterials in large quantities, and the efficiency of the manufacturing process can be improved.

[0083] Meanwhile, the guide portion (140) can guide the movement of the storage portion (100) when the storage portion (100) slides up and down. For example, the guide portion (140) can include a guide groove, and the storage portion can include a protrusion corresponding to the guide groove. Conversely, the guide portion (140) can include a protrusion, and the storage portion (100) can include a guide groove corresponding thereto.

[0084] Referring to FIG. 5 together with FIG. 1, the supply unit (200) may be located at the front end of the reaction unit (300). The supply unit (200) may accommodate one or more precursor units (20). Although FIG. 1 illustrates that the supply unit (200) accommodates one precursor unit (20), the present invention is not limited thereto, and multiple precursor units (20) may be accommodated in the supply unit (200).

[0085] The supply unit (200) may further include at least one pusher (210) for introducing a precursor unit (20) received from the receiving unit (200) into the reaction unit (300), a holder (215) for holding the at least one pusher (210), and a fixing unit (216) for preventing the pusher (210) from falling off the holder (215) when the at least one pusher (210) moves. A lubricant may be applied to the fixing unit (216) to facilitate smooth movement of the pusher (210).

[0086] In the step (S120) of introducing precursor units (20) into the reaction unit (300), at least one pusher (210) can slide in one direction (x, -x) to sequentially introduce the precursors (10) into the multiple chambers (330) of the reaction unit (300) one by one. That is, the precursors (10) of one row of precursor units (20) can be introduced into the reaction unit (300) simultaneously by the pusher (210).

[0087] The pusher (210) may include a main part (211) and a push part (213) provided at one end of the main part (211). The push part (213) may push the precursor (10) and inject the precursor (10) into the chamber (330).

[0088] The pusher (210) may further include a buffer member at the portion where the pusher (213) and the precursor (10) come into contact. Accordingly, the precursor (10) can be effectively prevented from being damaged or deformed during the process of introducing the precursor (10) into the chamber (330). The buffer member may include, for example, a sponge, but is not limited thereto.

[0089] Meanwhile, the pusher (210) may be arranged to face the inlet (310) of the chamber (330), and the pusher (210) may inject the precursor (10) into the chamber (330) in a bullet-like manner. Since the supply unit (200) uses the pusher (210) to individually inject the precursor (10) into the plurality of chambers (330) in a bullet-like manner, the precursors (10) can be quickly injected into the plurality of chambers (330) at a faster rate than the conventional method of injecting the precursor using a reaction module, thereby enabling the synthesis of boron nitride nanotubes in large quantities, and thus the efficiency of the manufacturing process can be improved.

[0090] Meanwhile, the inlet (310) of the chamber (330) may include a gate. As the gate is provided between the chamber (330) and the supply unit (200), after optimizing the temperature and gas atmosphere (e.g., nitrogen atmosphere) within the chamber (330), the precursor (10) can be supplied from the supply unit (200) into the chamber (330).

[0091] A vacuum pump may be installed in the supply unit (200), so that when the gate between the supply unit (200) and the chamber (330) is opened, the vacuum pump operates so that the reaction gas atmosphere and pressure of the supply unit (200) and the chamber (330) are matched, thereby transferring the precursor (10) from the supply unit (200) to the chamber (330) through the pusher (210), and closing the gate after the transfer.

[0092] Meanwhile, as illustrated in FIG. 5, the pusher (210) is provided with a plurality of corresponding pushers (210) for each chamber (330) to simultaneously push the precursors (10) into a plurality of chambers (330) arranged in parallel, one by one, so that the precursors (10) of one row of precursor units (20) can be simultaneously introduced into the reaction unit (300) in each chamber (330). That is, the pusher (210) can simultaneously push the precursors (10) of one row of precursor units (20) into the reaction unit (300).

[0093] As another example, as illustrated in FIG. 7, the pusher (210) may include a fork shape. For example, the pusher (210) may include a main portion (211), a plurality of sub-parts (212) branched from the main portion (211), and push portions (213) provided at one end of each of the sub-parts (211).

[0094] When the pusher (210) includes a fork shape, multiple precursors (10) can be simultaneously injected into multiple chambers (330) by operating only the main part (211) of the fork-shaped pusher (210) without having to operate multiple pushers (210) at once.

[0095] Meanwhile, the supply unit (200) may include various types of lifts to continuously supply a plurality of precursors (10) to a plurality of chambers (330). For example, when the supply unit (200) accommodates a plurality of precursors (10) in a vertical form, the lift may move in the vertical direction (z) to position the precursors (10) in front of at least one pusher (210) of the supply unit (200).

[0096] In addition, when the supply unit (200) accommodates a plurality of precursors (10) in a horizontal form, the lift may move horizontally to position the precursors (10) in front of at least one pusher (210) of the supply unit (200). In addition, when the precursors (10) are accommodated in the supply unit (200) on a circular orbit like a windmill, the lift may move circularly to position the precursors (10) in front of at least one pusher (210) of the supply unit (200).

[0097] Accordingly, the supply unit (200) can continuously supply precursors (10) in a row to the chamber (330). For example, the pusher (210) can inject the first precursor (10) into the chamber (330), position the second precursor (10) in front of the pusher (210), and then the pusher (210) can inject the second precursor (10) into the chamber (330). Through this, the boron nitride nanotube synthesis device (1000) can stably and quickly inject the precursors (10) into the chambers (330), thereby enabling mass production of nanomaterials at a faster rate.

[0098] Referring to FIGS. 8 and 9 together with FIG. 1, the reaction unit (300) may include a plurality of tubular chambers (330) arranged side by side and through which precursor units (20) move, a plurality of heaters (350) arranged on both sides of each chamber (330) and spaced apart from the chamber (330), and a temperature sensor (360) arranged in at least one chamber (330).

[0099] A plurality of chambers (330) can be arranged in parallel. Therefore, the synthesis of nanomaterials in large quantities can be possible, thereby improving the efficiency of the manufacturing process.

[0100] The chamber (330) has, for example, a cylindrical shape and can receive precursors (10) supplied from the supply unit (200). Thereafter, the chambers (330) can form nanomaterials (e.g., BNNT) on the precursors (10) in the second to fourth regions described below.

[0101] Additionally, a fastening portion or guide portion corresponding to the storage groove (12, 12') may be arranged in the chamber (330). As a result, the precursors (10) can move without falling out of the chamber (330).

[0102] Meanwhile, in the step (S130) of synthesizing nanomaterials (e.g., boron nitride nanotubes) by reacting the precursor units (20) and the reaction gas introduced into the reaction section (300), heat energy needs to be applied to the reaction section (300) in order to synthesize nanomaterials by reacting the precursors (10) and the reaction gas described later.

[0103] A plurality of heaters (350) can supply thermal energy to a chamber (330) through which precursors (10) pass and through which a reaction gas is supplied. At this time, the plurality of heaters (350) can be spaced apart from each other on both sides of each chamber (330) along the longitudinal direction of the chambers (330) to supply heat to the plurality of chambers (330). In addition, the plurality of heaters (350) can be connected to a controller that controls the plurality of heaters (350).

[0104] The temperature change rate over time of each chamber (330) of the reaction unit (300) may be 4°C to 9°C. If the temperature change rate over time of each chamber (330) is less than 4°C, the nanomaterial synthesis reaction needs to be performed for a long time. In addition, if the temperature change rate over time of each chamber (330) exceeds 9°C, the temperature of the chambers (330) of the reaction unit (300) may rapidly increase, and thus, there is a risk that the chambers (330) may be damaged by thermal shock.

[0105] Heat treatment for nanomaterial synthesis within the chamber (330) of the reaction unit (300) can be performed at a temperature range of 1100°C to 1700°C for 0.5 to 6 hours. The chamber (330) of the reaction unit (300) can use, for example, an alumina tube, but is not necessarily limited thereto, and can be formed of a heat-resistant material capable of withstanding temperatures up to approximately 1700°C.

[0106] Meanwhile, the reaction unit (300) may include a first region (Z1), a second region (Z2), and a third region (Z3) having different average temperatures. In this case, the average temperature of the third region (Z3) may be higher than the average temperature of the second region (Z2), and the average temperature of the second region (Z2) may be higher than the average temperature of the first region (Z1).

[0107] Additionally, the reaction unit (300) may further include a fourth region (Z4) and a fifth region (Z5) having different average temperatures and lower average temperatures than the third region (Z3). Specifically, the average temperature of the third region (Z3) may be higher than the average temperature of the fourth region (Z4), and the average temperature of the fourth region (Z4) may be higher than the average temperature of the fifth region (Z5).

[0108] That is, the temperature of the reaction unit (300) can sequentially increase from the first region (Z1) located near the inlet (310) connected to the supply unit, increase to the third region (Z3), and then sequentially decrease again to the fifth region (Z5). Through this, the temperature of the precursor (10) can increase gradually while passing from the first region (Z1) to the fifth region (Z5) without changing abruptly, and then gradually decrease again. As a result, the yield of the boron nitride nanotube synthesis device (1000) can be improved by preventing the precursor (10) from being damaged by thermal shock.

[0109] Specifically, the average temperature of the first region (Z1) may be 1000°C to 1300°C, the average temperature of the second region (Z2) may be 1100°C to 1400°C, the average temperature of the third region (Z3) may be 1200°C to 1700°C, the average temperature of the fourth region (Z4) may be 1200°C to 1500°C, and the average temperature of the fifth region (Z5) may be 1150°C to 1400°C.

[0110] Meanwhile, the reaction in which precursors (10) react with a reaction gas to synthesize nanomaterials may occur primarily in the third region (Z3) where the temperature is the highest. However, this is not limited to this, and the nanomaterial synthesis reaction may also occur in the second region (Z2) or the fourth region (Z4) which are close to the third region (Z3) and have a sufficiently high temperature.

[0111] The reaction unit (300) may include a temperature sensor (360) arranged in at least one chamber (330). Accordingly, the temperature sensor (360) precisely measures the temperature of each region, and allows the plurality of heaters (350) to supply thermal energy corresponding to the temperature range of each region to the first to fifth regions, thereby controlling the temperature of the reaction unit (300). However, the arrangement of the temperature sensor (360) is not limited thereto, and any arrangement is possible as long as the temperature of each region of the reaction unit (300) can be measured.

[0112] Meanwhile, each of the chambers (330) may be connected to two or more pipes (340) that supply reaction gas. The pipes (340) may directly supply reaction gas into the chamber (330) at a point between the two ends of the chamber (330). Accordingly, the consumption rate of reaction gas may be reduced and the synthesis efficiency of nanomaterials may be improved.

[0113] The pipes (340), each including a gas injection port (341) through which a reaction gas is injected, may be spaced apart from each other and arranged along the length direction of the chamber (330), as illustrated in FIG. 9. In addition, each of the pipes (340) may extend vertically through the chamber (330) from the upper portion of the chamber (330) and into the chamber (330). Accordingly, each of the pipes (340) may directly inject a reaction gas into the interior of the chamber (330).

[0114] In this way, by arranging multiple pipes (340) and directly injecting the reaction gas into the chamber (330), the concentration of the reaction gas reacting with the precursor (10) within the chamber (330) is maintained uniformly, thereby improving the synthesis efficiency of the nanomaterial.

[0115] The reaction gas may be, for example, a gas containing nitrogen, and nanomaterials may be synthesized on the inside and surface of the precursor (10) through the reaction between the precursor (10) and the reaction gas. For example, boron nitride nanotubes may be synthesized and grown on the inside and surface of the precursor (10). Nitrogen (N2) or ammonia (NH3) may be used as the reaction gas, and these may be mixed and supplied as a mixed gas. Alternatively, hydrogen (H2) may be additionally mixed and used.

[0116] At this time, the reaction gas may be supplied to the chamber (330) at a rate of 10 sccm to 1000 sccm. If the reaction gas is supplied at a rate of less than 10 sccm, the supply of nitrogen element is small, which reduces the efficiency of the boron nitridation reaction, and thus requires the reaction to be performed for a long time. In addition, if the rate of the reaction gas supplied to the chamber (330) exceeds 1000 sccm, the boron powder in the precursor may be ablated due to the rapid movement of the reaction gas, which may reduce the production yield of boron nitride nanotubes.

[0117] For example, when the reaction gas includes nitrogen (N2) or ammonia (NH3), the supply rate of nitrogen or ammonia may be 10 sccm to 1000 sccm. As another example, when the reaction gas includes hydrogen (H2), the supply rate of hydrogen may be 10 sccm to 100 sccm.

[0118] Meanwhile, the chamber (330) of the reaction unit (300) may include an inlet (310) connected to the supply unit (200) on one side and an outlet (320) connected to the discharge unit (400) on the other side. At this time, gates are installed in each of the inlet (310) and the discharge unit (320), so that the chamber (330) can be separated from the environments of the supply unit (200) and the discharge unit (400).

[0119] In addition, the boron nitride nanotube synthesis device (1000) may further include a vacuum processing unit. The vacuum processing unit is connected to the chamber (330) and can control the vacuum level inside the chamber (330). To this end, the vacuum processing unit may include a vacuum pump and a controller. The vacuum processing unit may be connected to an inlet (310) and / or an outlet (320).

[0120] Meanwhile, in the step (S140) of discharging from the reaction unit (300) to the discharge unit (400), the nanomaterials (e.g., boron nitride nanotubes) synthesized while passing through the reaction unit (300) can be discharged to the discharge unit (400) through the discharge port (320). At this time, the nanomaterials can freely fall through the discharge port (320) and be received in the discharge unit (400). Accordingly, a buffer member can be provided on the lower surface of the discharge unit (400). By providing the buffer member on the lower surface of the discharge unit (400), the nanomaterials freely falling from the chamber (330) to the discharge unit (400) can be effectively prevented from being damaged, broken, or deformed.

[0121] The synthesized nanomaterial can be stored in a storage unit (500) connected to a discharge unit (400). A large amount of nanomaterial can be stored in the storage unit (500). A discharge gate (410) is provided between the storage unit (500) and the discharge unit (400), so that when the discharge gate (410) is opened, the nanomaterial contained in the discharge unit (400) can be transferred to the storage unit (500). At this time, a buffer member can be provided on the lower surface of the storage unit (500). When all the nanomaterials are transferred to the storage unit (500), the discharge gate (410) provided between the storage unit (500) and the discharge unit (400) is closed, and the storage unit (500) is separated to recover the synthesized nanomaterial.

[0122] FIG. 10 is a perspective view schematically illustrating another example of a chamber and piping of the reaction unit of FIG. 8, FIG. 11 is a perspective view schematically illustrating another example of a chamber and piping of the reaction unit of FIG. 8, and FIG. 12 is a perspective view schematically illustrating another example of a chamber and piping of the reaction unit of FIG. 8.

[0123] Referring to FIGS. 10 to 12 together with FIG. 8, a reaction unit (300) according to embodiments of the present invention may include a plurality of tubular chambers (330) in which precursors (10) react with a reaction gas to synthesize nanomaterials, a plurality of heaters (350) arranged on both sides of each chamber (330) and spaced apart from the chamber (330), and a temperature sensor (360) arranged in at least one chamber (330).

[0124] The reaction unit (300) may include a first region (Z1), a second region (Z2), and a third region (Z3) having different average temperatures. In this case, the average temperature of the third region (Z3) may be higher than the average temperature of the second region (Z2), and the average temperature of the second region (Z2) may be higher than the average temperature of the first region (Z1).

[0125] Additionally, the reaction unit (300) may further include a fourth region (Z4) and a fifth region (Z5) having different average temperatures and lower average temperatures than the third region (Z3). Specifically, the average temperature of the third region (Z3) may be higher than the average temperature of the fourth region (Z4), and the average temperature of the fourth region (Z4) may be higher than the average temperature of the fifth region (Z5).

[0126] Meanwhile, each of the chambers (330) may be connected to two or more pipes (340, 340a, 340b) that supply reaction gas. In addition, each of the pipes (340, 340a, 340b) may include a gas injection port (341, 341a, 341b) through which the reaction gas is injected. The gas injection port (341, 341a, 341b) may include an opening through which the reaction gas is injected into the chamber (330).

[0127] Referring to FIG. 10, the pipes (340) may be spaced apart from each other and arranged along the length of the chamber (330). At this time, each of the pipes (340) may extend into the chamber (330) by vertically penetrating the chamber (330) from the upper portion of the chamber (330) and the lower portion of the chamber (330). Accordingly, each of the pipes (340) may directly inject a reaction gas into the interior of the chamber (330).

[0128] In this way, a plurality of pipes (340) are arranged in the upper part of the chamber (330) and the lower part of the chamber (330) along the longitudinal direction of the chamber (330), and by directly injecting the reaction gas into the chamber (330), the concentration of the reaction gas that reacts with the precursor (10) within the chamber (330) is maintained uniformly, thereby improving the synthesis efficiency of the nanomaterial.

[0129] Referring to FIG. 11, each of the pipes (340a) may be directly positioned within the chamber (330) along the longitudinal direction of the chamber (330) at the upper portion of the chamber (330) and the lower portion of the chamber (330). At this time, gas injection holes (341a) spaced apart from each other by a certain distance may be positioned in each of the pipes (340a). Accordingly, each of the pipes (340a) may directly inject a reaction gas into the interior of the chamber (330).

[0130] In this way, a plurality of pipes (340a) are arranged in the upper part of the chamber (330) and the lower part of the chamber (330) along the longitudinal direction of the chamber (330), and gas injection holes (341a) spaced apart from each other are arranged in each pipe (340a), and thus, by directly injecting the reaction gas into the chamber (330), the concentration of the reaction gas that reacts with the precursor (10) within the chamber (330) is maintained uniformly, so that the synthesis efficiency of the nanomaterial can be improved.

[0131] Referring to FIG. 12, each of the plurality of gas injection ports (341b) included in the pipe (340b) may include an inclined surface so that the area of ​​the opening of the gas injection port (341b) becomes narrower when directed from inside the chamber (330) to outside the chamber (330). As a result, when the reaction gas is injected into the chamber (330), a vortex due to expansion of the reaction gas can be prevented, and particles generated during the reaction can be prevented from accumulating in the gas injection port (341b) and clogging the opening of the gas injection port (341b), thereby improving the synthesis efficiency of nanomaterials.

[0132] Although the present invention has been described above with reference to limited embodiments and drawings, the present invention is not limited thereto, and it is obvious that various modifications and variations are possible within the scope of the technical idea of ​​the present invention and the equivalent scope of the patent claims to be described below by a person having ordinary skill in the art to which the present invention pertains.

Claims

1. A storage unit for accommodating precursor units forming a plurality of rows, each of which includes a plurality of precursors; A reaction unit that receives the precursor units stored in the storage unit and synthesizes nano materials from the precursors; and A supply unit connected to the storage unit and the reaction unit, and receiving the precursor units one by one from the storage unit and supplying them to the reaction unit; The above reaction unit includes a plurality of tubular chambers into which the precursors of the above precursor units are simultaneously injected, The above reaction section includes at least one heater and a first zone, a second zone and a third zone having different average temperatures, A boron nitride nanotube synthesis device wherein the average temperature of the third region is higher than the average temperatures of the first region and the second region.

2. In paragraph 1, The above precursor is a boron nitride nanotube synthesis device which is a precursor for synthesizing boron nitride nanotubes.

3. In paragraph 1, A boron nitride nanotube synthesis device, wherein the supply unit includes at least one pusher for introducing the precursor units into the reaction unit.

4. In paragraph 3, The above pusher is a boron nitride nanotube synthesis device that simultaneously pushes the precursors of the above one row of precursor units.

5. In paragraph 1, The above storage unit is a boron nitride nanotube synthesis device that can slide up and down.

6. In paragraph 5, A boron nitride nanotube synthesis device including a guide part on the outer surface of the storage part for guiding the movement of the storage part.

7. In paragraph 1, A device for synthesizing boron nitride nanotubes, each of the above chambers being connected to two or more pipes supplying reaction gases.

8. In paragraph 1, A boron nitride nanotube synthesis device, wherein the reaction section further includes a fourth region and a fifth region having different average temperatures than the third region.

9. A step of delivering precursor units forming a plurality of rows, each including a plurality of precursors, to a supply unit; A step of simultaneously introducing the precursors of one row precursor unit into the reaction section by a pusher; A step of synthesizing nanomaterials by reacting the precursor units and the reaction gas introduced into the reaction unit in the reaction unit; and A step of discharging the synthesized nano material from the reaction unit to the discharge unit; The above reaction unit includes a plurality of tubular chambers into which the precursors of the above precursor units are simultaneously injected, The above reaction section includes at least one heater and a first zone, a second zone and a third zone having different average temperatures, A method for synthesizing boron nitride nanotubes, wherein the average temperature of the third region is higher than the average temperature of the second region.

10. In paragraph 9, A method for synthesizing boron nitride nanotubes, wherein the rate of change in temperature over time of the above reaction section is 4°C / min to 9°C / min.

11. In paragraph 9, A method for synthesizing boron nitride nanotubes, wherein each of the above chambers is connected to two or more pipes supplying reaction gas.

12. In paragraph 9, At the stage of delivery to the above supply department, The above storage section slides in the direction of the supply section, A method for synthesizing boron nitride nanotubes by delivering the above precursor units to the above supply unit.

13. In paragraph 12, When all of the precursor units stored in the above storage unit are supplied to the supply unit, A method for synthesizing boron nitride nanotubes, wherein the receiving portion slides in the opposite direction to the supply portion.

14. In paragraph 9, A method for synthesizing boron nitride nanotubes in which the nanomaterial is synthesized in the third region.

15. In paragraph 9, A method for synthesizing boron nitride nanotubes, wherein the reaction section further includes a fourth region and a fifth region having different average temperatures and having a lower average temperature than the third region.

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