An apparatus and method for producing 6n high purity boron

Abstract

The application discloses a device and method for preparing 6N high-purity boron, wherein the device for preparing 6N high-purity boron comprises a raw material storage mechanism, a hydrogen gas conveying mechanism and a reduction reaction mechanism; the raw material storage mechanism is used for storing boron tribromide, the hydrogen gas conveying mechanism is used for conveying hydrogen gas, and the raw material storage mechanism is connected with the hydrogen gas conveying mechanism and the reduction reaction mechanism in communication, so that the boron tribromide and the hydrogen gas can enter the reduction reaction mechanism to perform a reduction reaction; the reduction reaction mechanism at least comprises a preheating section and a reduction reaction section, the preheating section and the reduction reaction section are connected in communication, the boron tribromide and the hydrogen gas can be mixed into a mixed gas in the preheating section, the mixed gas can enter the reduction reaction section and perform a reduction reaction in the reduction reaction section to form 6N high-purity boron. The device not only greatly improves the reaction rate in the preparation process of high-purity boron, but also effectively improves the stability of boron purity.

Description

Technical Field

[0001] This invention relates to the field of boron preparation technology, and in particular to an apparatus and method for preparing 6N high-purity boron. Background Technology

[0002] High-purity boron plays a vital role in capacitor manufacturing, electronic components, the nuclear industry, and the metallurgical industry, and can be used as a structural material in rockets. Currently, the preparation of high-purity boron with a purity of 6N and above in China generally suffers from technical defects such as equipment corrosion, slow reaction rates, and unstable boron purity.

[0003] Therefore, how to improve the reaction rate in the preparation process of high-purity boron and enhance the stability of boron purity are technical problems that urgently need to be solved by those skilled in the art. Summary of the Invention

[0004] In view of this, the object of the present invention is to provide an apparatus for preparing 6N high-purity boron, which can improve the reaction rate in the preparation process of high-purity boron and improve the stability of boron purity.

[0005] Another object of the present invention is to provide a method for preparing 6N high-purity boron.

[0006] To achieve the above objectives, the present invention provides the following technical solution: An apparatus for preparing 6N high-purity boron includes a raw material storage mechanism, a hydrogen delivery mechanism, and a reduction reaction mechanism; The raw material storage mechanism is used to store boron tribromide, and the hydrogen conveying mechanism is used to convey hydrogen. The raw material storage mechanism is connected to the hydrogen conveying mechanism and the reduction reaction mechanism respectively, so that the boron tribromide and the hydrogen can enter the reduction reaction mechanism to carry out the reduction reaction. The reduction reaction mechanism includes at least a preheating section and a reduction reaction section, which are connected to each other. The boron tribromide and the hydrogen gas can be mixed in the preheating section to form a mixed gas. The mixed gas can enter the reduction reaction section and undergo a reduction reaction to form 6N high-purity boron.

[0007] Optionally, the reaction mechanism further includes a cooling section, which is connected to the reduction reaction section, and the preheating section, the reduction reaction section, and the cooling section are arranged sequentially from the position closest to the raw material storage mechanism to the position furthest from the raw material storage mechanism; The cooling section is capable of cooling the boron tribromide that has not fully reacted in the reduction reaction section.

[0008] Optionally, the raw material storage mechanism includes a raw material bottle and a rate regulator, wherein the raw material bottle is connected to the reduction reaction mechanism via a first connecting pipe; The raw material bottle is used to store the boron tribromide, and the rate regulator is disposed inside the raw material bottle to regulate the rate at which the boron tribromide enters the reduction reaction mechanism.

[0009] Optionally, the preset delivery rate of the rate regulator is 1 ml / s to 3 ml / s.

[0010] Optionally, the hydrogen delivery mechanism includes a hydrogen delivery pipeline and a hydrogen valve, wherein the hydrogen valve is disposed on the hydrogen delivery pipeline to control the opening and closing of the hydrogen delivery pipeline.

[0011] Optionally, a Dewar flask is also included, which is connected to the cooling section via a third connecting pipe, and the Dewar flask is used to receive the boron tribromide output from the cooling section.

[0012] Optionally, the connection end between the Dewar canister and the third connecting pipe is also equipped with a sponge palladium detection mechanism for detecting whether hydrogen is leaking.

[0013] Optionally, a leak detection mechanism may also be included, which includes an argon gas delivery pipeline and an argon gas valve. The argon gas valve is located on the argon gas delivery pipeline to control the opening and closing of the argon gas delivery pipeline.

[0014] Optionally, the reduction reaction mechanism is connected to the hydrogen delivery mechanism and the leak detection mechanism via a third connecting pipe.

[0015] Optionally, the reduction reaction mechanism is a tubular structure, the preheating section includes a preheating tube body and a heating element disposed on the tube wall of the preheating tube body, the preheating tube body is connected to the second connecting pipe, a spiral gas conveying assembly is disposed inside the preheating tube body, and the first connecting pipe is connected to the spiral gas conveying assembly. The reduction reaction section includes a reaction tube and a heating wire disposed inside the reaction tube, the heating wire being connected to a power source; The cooling section includes a cooling pipe body and a silicone tube disposed on the wall of the cooling pipe body; A T-joint is provided between the preheating section and the reduction reaction section. The first port of the T-joint is connected to the reduction reaction section, the second port of the T-joint is connected to the second connecting pipeline, and the third port of the T-joint is connected to the spiral gas conveying assembly.

[0016] Optionally, the heating wire is a tantalum wire with a purity of 99.9%, a diameter of 1mm-2mm, and a length 1cm-2cm shorter than the length of the reduction reaction section.

[0017] Optionally, the reduction reaction mechanism is made of silicon dioxide.

[0018] A method for preparing 6N high-purity boron, applied in the apparatus for preparing 6N high-purity boron disclosed in any of the above embodiments, includes the following steps: S100: Activate the cooling assembly of the Dewar canister to bring the outer surface temperature of the Dewar canister to a first preset temperature; S200: Turn on the first switch of the preheating section in the reduction reaction mechanism so that the temperature of the preheating section reaches the second preset temperature. When the temperature of the preheating section reaches the second preset temperature, turn on the second switch of the reduction reaction section in the reduction reaction mechanism so that the temperature of the preheating section reaches the third preset temperature, and keep the voltage constant. S300: The rate regulator is activated to deliver boron tribromide to the preheating section of the reduction reaction mechanism. At the same time, the hydrogen valve is opened, allowing the hydrogen in the hydrogen delivery mechanism to enter the preheating section of the reduction reaction mechanism and mix with the boron tribromide to form a mixed gas. The mixed gas enters the reduction reaction section of the reduction reaction mechanism to generate 6N high-purity boron. The unreacted boron tribromide enters the cooling section of the reduction reaction mechanism for cooling. S400: Turn off the cooling components of the Dewar canister, turn off the heating switch of the preheating section and the first switch of the reaction section in the reduction reaction mechanism, continue to introduce hydrogen for a preset time, and observe whether the sponge palladium detection mechanism expands. When the sponge palladium detection mechanism does not expand, open the argon valve and close the hydrogen valve until the room temperature is reached in the reduction reaction mechanism, then close the argon valve. S500: Collect the 6N high-purity boron.

[0019] Optionally, before step S100, the method further includes: checking the apparatus for preparing 6N high-purity boron for leaks; if the test is qualified, checking whether the silicone tube in the cooling zone of the reduction reaction mechanism is attached to the cooling zone.

[0020] Optionally, the first preset temperature is 25℃-30℃, the second preset temperature is 95℃-100℃, and the third preset temperature is 1200℃-1300℃.

[0021] Optionally, step S500 specifically includes: S501: Wrap the heating wire and the 6N high-purity boron attached to the heating wire in a dust-free bag, and separate the heating wire and the 6N high-purity boron from the reduction reaction section using an ultrasonic cutting blade; S502: Break the 6N high-purity boron attached to the heating wire and separate the 6N high-purity boron from the heating wire.

[0022] Optionally, the method further includes step S600, which involves using the water displacement method to detect the density of the separated 6N high-purity boron and the heating wire product to determine the purity of the 6N high-purity boron.

[0023] As can be seen from the above technical solution, when preparing 6N high-purity boron, boron tribromide stored in the raw material storage device needs to be transported to the reduction reaction device. At the same time, hydrogen gas is transported through the hydrogen gas transport device to the preheating section of the reduction reaction device to mix with boron tribromide to form a mixed gas. After the mixed gas enters the reduction reaction section, a reduction reaction is carried out in the reduction reaction section to form 6N high-purity boron.

[0024] Compared with the prior art, the apparatus for preparing 6N high-purity boron disclosed in the embodiments of the present invention, by using boron tribromide to react with hydrogen and setting up a preheating section and a reduction reaction section, not only greatly improves the reaction rate in the preparation process of high-purity boron, but also effectively improves the stability of boron purity. Attached Figure Description

[0025] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art are briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the provided drawings without creative effort.

[0026] Figure 1 This is a schematic diagram of the overall structure of the apparatus for preparing 6N high-purity boron disclosed in the embodiments of the present invention; Figure 2 This is a schematic diagram of the method for preparing 6N high-purity boron disclosed in an embodiment of the present invention.

[0027] The names of the components are as follows: 100. Raw material storage mechanism; 101. Raw material bottle; 102. Rate regulator; 200. Hydrogen delivery mechanism; 201. Hydrogen delivery pipeline; 202. Hydrogen valve; 300. Reduction reaction mechanism; 301. Preheating section; 302. Reduction reaction section; 303. Cooling section; 304. Heating element; 305. Spiral gas delivery assembly; 306. Heating wire; 307. Power supply; 308. Silicone tubing; 309. T-connector; 400. Dewar flask; 500. Leak detection mechanism; 501. Argon delivery pipeline; 502. Argon valve; 600. First connecting pipeline; 700. Second connecting pipeline; 800. Third connecting pipeline; 900. Sponge palladium detection mechanism. Detailed Implementation

[0028] In view of this, the core of the present invention is to provide an apparatus for preparing 6N high-purity boron, which can improve the reaction rate in the preparation process of high-purity boron and improve the stability of boron purity.

[0029] Another core aspect of this invention lies in providing a method for preparing 6N high-purity boron.

[0030] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0031] Please refer to Figure 1-2 ,in, Figure 1 This is a schematic diagram of the overall structure of the apparatus for preparing 6N high-purity boron disclosed in the embodiments of the present invention; Figure 2 This is a schematic diagram of the method for preparing 6N high-purity boron disclosed in an embodiment of the present invention.

[0032] The apparatus for preparing 6N high-purity boron disclosed in this invention includes a raw material storage mechanism 100, a hydrogen delivery mechanism 200, and a reduction reaction mechanism 300. The raw material storage mechanism 100 stores boron tribromide, and the hydrogen delivery mechanism 200 delivers hydrogen gas. The raw material storage mechanism 100 is connected to both the hydrogen delivery mechanism 200 and the reduction reaction mechanism 300, allowing boron tribromide and hydrogen gas to enter the reduction reaction mechanism 300 for a reduction reaction.

[0033] The reduction reaction mechanism 300 includes at least a preheating section 301 and a reduction reaction section 302, which are connected. Boron tribromide and hydrogen can be mixed in the preheating section 301 to form a mixed gas. The mixed gas can enter the reduction reaction section 302 and undergo a reduction reaction to form 6N high-purity boron.

[0034] When preparing 6N high-purity boron, boron tribromide stored in the raw material storage unit 100 needs to be transported to the reduction reaction unit 300. At the same time, hydrogen gas is transported through the hydrogen gas transport unit 200 to the preheating section 301 of the reduction reaction unit 300 to mix with boron tribromide to form a mixed gas. After the mixed gas enters the reduction reaction section 302, a reduction reaction is carried out in the reduction reaction section 302 to form 6N high-purity boron.

[0035] Compared with the prior art, the apparatus for preparing 6N high-purity boron disclosed in the embodiments of the present invention, by using boron tribromide to react with hydrogen and setting up a preheating section and a reduction reaction section, not only greatly improves the reaction rate in the preparation process of high-purity boron, but also effectively improves the stability of boron purity.

[0036] It should be noted that the Gibbs free energy of the reaction between boron tribromide and hydrogen is less than 0 and has a very high absolute value, meaning that the reaction has a strong tendency to proceed spontaneously, and is therefore faster than other methods for preparing high-purity boron.

[0037] The boron tribromide disclosed in the embodiments of the present invention is preferably 4N boron tribromide.

[0038] As a further embodiment, the reduction reaction mechanism 300 disclosed in this embodiment of the invention further includes a cooling section 303, wherein the cooling section 303 is connected to the reduction reaction section 302, and the preheating section 301, the reduction reaction section 302 and the cooling section 303 are arranged sequentially from the position close to the raw material storage mechanism 100 to the position far away from the raw material storage mechanism 100.

[0039] It should be noted that the cooling section 303 can cool the boron tribromide that has not completely reacted in the reduction reaction section 302.

[0040] The embodiments of the present invention do not limit the specific structure of the raw material storage mechanism 100. Any structure that meets the requirements of the present invention is within the protection scope of the present invention.

[0041] As one possible embodiment, the raw material storage mechanism 100 disclosed in this embodiment of the invention includes a raw material bottle 101 and a rate regulator 102, wherein the raw material bottle 101 is connected to the reduction reaction mechanism 300 through a first connecting pipe 600.

[0042] The raw material bottle 101 is used to store boron tribromide, and the rate regulator 102 is installed inside the raw material bottle 101 to regulate the rate at which boron tribromide enters the reduction reaction mechanism 300.

[0043] When the rate regulator 102 is turned on, boron tribromide in the raw material bottle 101 will enter the preheating section 301 of the reduction reaction mechanism 300 through the first connecting pipe 600 at a preset delivery rate.

[0044] The embodiments of the present invention do not limit the preset delivery rate of boron tribromide. Any preset delivery rate that meets the requirements of the present invention is within the protection scope of the present invention.

[0045] As one possible embodiment, the preset delivery rate of the rate regulator 102 disclosed in this embodiment of the invention is 1 ml / s-3 ml / s. When boron tribromide enters the preheating section 301 of the reduction reaction mechanism 300 at a constant rate, the mixing uniformity of boron tribromide and hydrogen can be improved, avoiding material waste caused by uneven mixing, thus saving costs and increasing the reaction rate.

[0046] The specific structure of the hydrogen delivery mechanism 200 is not limited in the embodiments of the present invention. As long as the preset delivery rate meets the requirements of the present invention, it is within the protection scope of the present invention.

[0047] As one possible embodiment, the hydrogen delivery mechanism 200 disclosed in this embodiment of the invention includes a hydrogen delivery pipeline 201 and a hydrogen valve 202, wherein the hydrogen valve 202 is disposed on the hydrogen delivery pipeline 201 to control the opening and closing of the hydrogen delivery pipeline 201. When the hydrogen valve 202 is opened, hydrogen can enter the preheating zone in the reduction reaction mechanism 300 from the hydrogen delivery pipeline 201.

[0048] In order to recover and utilize the unreacted boron tribromide, the apparatus for preparing 6N high-purity boron disclosed in the embodiments of the present invention further includes a Dewar jar 400, wherein the Dewar jar 400 is connected to the cooling section 303 through a third connecting pipe 800, and the Dewar jar 400 is used to receive the boron tribromide output from the cooling section 303.

[0049] It should be noted that the Dewar 400 has a cooling component, and boron tribromide can continue to be cooled and liquefied within the Dewar 400 for easy recycling.

[0050] The connection end between the Dewar canister 400 and the third connecting pipe 800 is also equipped with a sponge palladium detection mechanism 900 for detecting whether hydrogen is leaking.

[0051] When hydrogen leaks, the sponge palladium detection mechanism 900 will expand, at which point the connection between the Dewar canister 400 and the third connecting pipe 800 needs to be inspected.

[0052] To detect whether there are leaks at the connections between the raw material storage mechanism 100 and the reduction reaction mechanism 300, and between the hydrogen delivery mechanism 200 and the reduction reaction mechanism 300 in the apparatus for preparing 6N high-purity boron, the apparatus for preparing 6N high-purity boron disclosed in this embodiment of the invention further includes a leak detection mechanism 500. The leak detection mechanism 500 includes an argon gas delivery pipeline 501 and an argon gas valve 502. The argon gas valve 502 is disposed on the argon gas delivery pipeline 501 to control the opening and closing of the argon gas delivery pipeline 501.

[0053] Before the reduction reaction is carried out in the apparatus for preparing 6N high-purity boron, soapy water should be applied to all the connections in the apparatus. Then, the argon valve 502 should be opened to deliver argon gas through the argon gas delivery pipeline 501 into the entire apparatus for preparing 6N high-purity boron. Observe whether bubbles are generated to check for leaks.

[0054] It should be noted that the reduction reaction mechanism 300 is connected to the hydrogen delivery mechanism 200 and the leak detection mechanism 500 through the second connecting pipe 700.

[0055] The embodiments of the present invention do not limit the specific structure of the preheating section 301, the reduction reaction section 302 and the cooling section 303. Any structure that meets the requirements of the present invention is within the protection scope of the present invention.

[0056] Specifically, the reduction reaction mechanism 300 disclosed in this embodiment of the invention is a tubular structure. The preheating section 301 includes a preheating tube and a heating element 304 disposed on the tube wall of the preheating tube. The preheating tube is connected to the second connecting pipe 700. A spiral gas conveying assembly 305 is disposed inside the preheating tube. The first connecting pipe 600 is connected to the spiral gas conveying assembly 305.

[0057] Hydrogen enters the preheating tube body from the hydrogen delivery pipeline 201 through the second connecting pipe 700. At the same time, boron tribromide enters the spiral gas delivery assembly 305 in the preheating tube body through the first connecting pipe 600. The heating element 304 is turned on to vaporize the boron tribromide in the spiral gas delivery assembly 305. The vaporized boron tribromide and hydrogen are mixed to form a mixed gas.

[0058] Specifically, the reduction reaction section 302 includes a reaction tube and a heating wire 306 disposed within the reaction tube, wherein the heating wire 306 is connected to a power supply 307.

[0059] In this process, the mixed gas, after being heated in the preheating tube, enters the reduction reaction section 302. The power supply 307 is turned on to heat the heating wire 306. When the temperature reaches the second preset temperature, the mixed gas generates 6N high-purity boron that adheres to the heating wire 306.

[0060] Specifically, the cooling section 303 includes a cooling tube body and a silicone tube 308 disposed on the tube wall of the cooling tube body. The silicone tube can cool the cooling tube body. Boron tribromide that has not fully reacted in the reduction reaction section 302 enters the cooling section 303 for cooling, so as to be recycled.

[0061] It should be noted that a T-junction 309 is provided between the preheating section 301 and the reduction reaction section 302. The first port of the T-junction 309 is connected to the reduction reaction section 302, the second port of the T-junction 309 is connected to the second connecting pipe 700, and the third port of the T-junction 309 is connected to one end of the spiral gas conveying assembly 305. The other end of the spiral gas conveying assembly 305 is connected to the first connecting pipe 600. Boron tribromide enters the spiral gas conveying assembly 305 from the first connecting pipe 600, is vaporized, and then enters the third port of the T-junction 309. Hydrogen enters the second port of the T-junction 309 from the second connecting pipe 700. The vaporized boron tribromide and hydrogen mix and then enter the reduction reaction section 302 from the first port of the T-junction 309.

[0062] The embodiments of the present invention do not limit the specific material of the reduction reaction mechanism 300. Any structure that meets the requirements of the present invention is within the protection scope of the present invention.

[0063] As one possible embodiment, the reduction reaction mechanism 300 disclosed in this embodiment of the invention is made of silicon dioxide.

[0064] The embodiments of the present invention do not limit the specific material and structure of the heating wire 306. Any structure that meets the requirements of the present invention is within the protection scope of the present invention.

[0065] As one possible embodiment, the heating wire 306 disclosed in this embodiment of the invention is a tantalum wire, wherein the purity of the tantalum wire is 99.9%, the diameter of the tantalum wire is 1mm-2mm, and the length of the tantalum wire is 1cm-2cm shorter than the length of the reduction reaction section 302.

[0066] The tantalum wire disclosed in this invention replaces the traditional tungsten wire. Tantalum wire has more stable physical properties at high temperatures. Experiments have shown that when a tungsten wire is removed from a quartz tube, it breaks into several pieces, while tantalum wire does not exhibit this problem. Moreover, high-purity tantalum wire is cheaper than high-purity tungsten wire, which is more conducive to cost control.

[0067] The embodiments of the present invention do not limit the specific material of the reduction reaction mechanism 300. Any material that meets the requirements of the present invention is within the protection scope of the present invention.

[0068] Preferably, the reduction reaction mechanism 300 disclosed in the embodiments of the present invention is made of silicon dioxide.

[0069] With this setup, silicon dioxide will not react with boron tribromide, and tantalum wire is a disposable tool, meaning that a new tantalum wire is used for each production run, thus avoiding the corresponding equipment corrosion problems.

[0070] This invention also discloses a method for preparing 6N high-purity boron, comprising the following steps: S100: Activate the cooling components of the Dewar 400 to bring the outer surface temperature of the Dewar 400 to the first preset temperature; S200: Turn on the first switch of the preheating section 301 in the reduction reaction mechanism 300 so that the temperature of the preheating section 301 reaches the second preset temperature. When the temperature of the preheating section 301 reaches the second preset temperature, turn on the second switch of the reduction reaction section 302 in the reduction reaction mechanism 300 so that the temperature of the preheating section 301 reaches the third preset temperature, and keep the voltage constant. S300: The rate regulator 102 is turned on to deliver boron tribromide to the preheating section 301 in the reduction reaction mechanism 300. At the same time, the hydrogen valve 202 is turned on, so that the hydrogen in the hydrogen delivery mechanism 200 enters the preheating section 301 in the reduction reaction mechanism 300 and mixes with boron tribromide to form a mixed gas. The mixed gas enters the reduction reaction section 302 in the reduction reaction mechanism 300 to generate 6N high-purity boron. The unreacted boron tribromide enters the cooling section 303 in the reduction reaction mechanism 300 for cooling. S400: Turn off the cooling components of the Dewar 400, turn off the first switch of the preheating section 301 and the second switch of the reduction reaction section 302 in the reduction reaction mechanism 300, continue to introduce hydrogen for a preset time, and observe whether the sponge palladium detection mechanism 900 expands. When no expansion occurs in the sponge palladium detection mechanism 900, open the argon valve 502 and close the hydrogen valve 202 until the reduction reaction mechanism 300 reaches room temperature, then close the argon valve 502. S500: Collects 6N high-purity boron.

[0071] It should be noted that before step S100, the following steps are also included: checking whether the apparatus for preparing 6N high-purity boron has any leaks. If the test is qualified, checking whether the silicone tube 308 of the cooling zone of the reduction reaction mechanism 300 is attached to the cooling zone section 303.

[0072] It should be further noted that the first preset temperature is 25℃-30℃, the second preset temperature is 95℃-100℃, and the third preset temperature is 1200℃-1300℃.

[0073] When preparing 6N high-purity boron, firstly, check the apparatus for leaks. If the leak is detected, check if the silicone tube 308 in the cooling zone of the reduction reaction mechanism 300 is attached to the cooling zone. Then, start the cooling assembly of the Dewar jar 400. When the outer surface temperature of the Dewar jar 400 reaches the first preset temperature of 25℃-30℃, open the first switch of the preheating section 301 in the reduction reaction mechanism 300, allowing the temperature of the preheating section 301 to reach 95℃-100℃. When the temperature of the preheating section 301 reaches 95℃-100℃, open the reduction reaction section 30... The second switch 2 causes the temperature of the preheating section 301 to reach 1200℃-1300℃ while maintaining a constant voltage. Then, the rate regulator 102 is activated to deliver boron tribromide to the preheating section 301 in the reduction reaction mechanism 300. At the same time, the hydrogen valve 202 is opened, allowing the hydrogen in the hydrogen delivery mechanism 200 to enter the preheating section 301 in the reduction reaction mechanism 300 and mix with the boron tribromide to form a mixed gas. The mixed gas enters the reduction reaction section 302 in the reduction reaction mechanism 300 to generate 6N high-purity boron. The unreacted boron tribromide enters the cooling section 303 in the reduction reaction mechanism 300 for cooling. When the thickness of the 6N high-purity boron deposited on the tantalum wire reaches 4mm-6mm, turn off the cooling components of the Dewar jar 400, turn off the first switch of the preheating section 301 and the second switch of the reduction reaction section 302 in the reduction reaction mechanism 300, and continue to introduce hydrogen gas for 20min-30min. At the same time, observe whether the sponge palladium detection mechanism 900 expands. When no expansion occurs in the sponge palladium detection mechanism 900, open the argon valve 502 and close the hydrogen valve 202 until the reduction reaction mechanism 300 reaches room temperature. Then close the argon valve 502 and finally collect the 6N high-purity boron.

[0074] It should be noted that step S500 specifically includes: S501: Wrap the heating wire 306 and the 6N high-purity boron attached to the heating wire 306 with a dust-free bag, and separate the heating wire 306 and the 6N high-purity boron from the reduction reaction section 302 using an ultrasonic cutting blade; S502: Crush the 6N high-purity boron attached to the heating wire 306 and separate the 6N high-purity boron from the heating wire 306.

[0075] In order to detect whether the purity of the high-purity boron prepared by the above-mentioned device meets the standard, the method for preparing 6N high-purity boron disclosed in the embodiments of the present invention further includes step S600, which involves using the water displacement method to detect the density of the product of the divided 6N high-purity boron and the heating wire 306 to determine the purity of the 6N high-purity boron.

[0076] Specifically, take equal volumes of standard high-purity boron powder and tantalum powder with a purity of 99.9%, and weigh them. If the mass of the collected 6N high-purity boron product is close to that of the same volume of standard high-purity boron powder but less than that of the same volume of tantalum powder with a purity of 99.9%, then the collected 6N high-purity boron product can be considered qualified. If the collected 6N high-purity boron product deviates significantly from the data of the standard high-purity boron powder, then the suspected tantalum wire residue should be removed with a glass rod until the mass of the collected 6N high-purity boron product is close to that of the standard high-purity boron powder.

[0077] Finally, it should be noted that in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the term "comprising" or any other variation thereof is intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus.

[0078] The various embodiments in this specification are described in a progressive manner, with each embodiment focusing on the differences from other embodiments. The same or similar parts between the various embodiments can be referred to each other.

[0079] The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. An apparatus for preparing 6N high-purity boron, characterized in that, This includes raw material storage facilities, hydrogen delivery facilities, and reduction reaction facilities; The raw material storage mechanism is used to store boron tribromide, and the hydrogen conveying mechanism is used to convey hydrogen. The raw material storage mechanism and the hydrogen conveying mechanism are respectively connected to the reduction reaction mechanism so that the boron tribromide and the hydrogen can enter the reduction reaction mechanism to carry out the reduction reaction. The reduction reaction mechanism includes at least a preheating section and a reduction reaction section, which are connected to each other. The boron tribromide and the hydrogen can be mixed in the preheating section to form a mixed gas. The mixed gas can enter the reduction reaction section and undergo a reduction reaction to form 6N high-purity boron. The preheating section includes a preheating pipe body and a heating element disposed on the pipe wall of the preheating pipe body, and a spiral gas conveying assembly is disposed inside the preheating pipe body; The raw material storage mechanism includes a raw material bottle and a rate regulator. The raw material bottle is connected to the spiral gas conveying assembly through a first connecting pipe. The raw material bottle is used to store the boron tribromide, and the rate regulator is disposed inside the raw material bottle to regulate the rate at which the boron tribromide enters the reduction reaction mechanism; The reduction reaction mechanism is connected to the hydrogen delivery mechanism and the leak detection mechanism respectively through the second connecting pipe; A tee connector is provided between the preheating section and the reduction reaction section. The first port of the tee connector is connected to the reduction reaction section, the second port of the tee connector is connected to the second connecting pipeline, the third port of the tee connector is connected to the spiral gas conveying assembly, and the preheating pipe body is connected to the second connecting pipeline.

2. The apparatus for preparing 6N high-purity boron according to claim 1, characterized in that, The reduction reaction mechanism further includes a cooling section, which is connected to the reduction reaction section, and the preheating section, the reduction reaction section, and the cooling section are arranged sequentially from the position closest to the raw material storage mechanism to the position furthest from the raw material storage mechanism; The cooling section is capable of cooling the boron tribromide that has not fully reacted in the reduction reaction section.

3. The apparatus for preparing 6N high-purity boron according to claim 1, characterized in that, The preset delivery rate of the rate regulator is 1 ml / s-3 ml / s.

4. The apparatus for preparing 6N high-purity boron according to claim 1, characterized in that, The hydrogen delivery mechanism includes a hydrogen delivery pipeline and a hydrogen valve. The hydrogen valve is located on the hydrogen delivery pipeline to control the opening and closing of the hydrogen delivery pipeline.

5. The apparatus for preparing 6N high-purity boron according to claim 2, characterized in that, It also includes a Dewar flask, which is connected to the cooling section via a third connecting pipe, and the Dewar flask is used to receive the boron tribromide output from the cooling section.

6. The apparatus for preparing 6N high-purity boron according to claim 5, characterized in that, The connection end between the Dewar canister and the third connecting pipeline is also equipped with a sponge palladium detection mechanism for detecting whether hydrogen is leaking.

7. The apparatus for preparing 6N high-purity boron according to claim 6, characterized in that, It also includes a leak detection mechanism, which includes an argon gas delivery pipeline and an argon gas valve. The argon gas valve is installed on the argon gas delivery pipeline to control the opening and closing of the argon gas delivery pipeline.

8. The apparatus for preparing 6N high-purity boron according to claim 7, characterized in that, The reduction reaction mechanism is a tubular structure; The reduction reaction section includes a reaction tube and a heating wire disposed inside the reaction tube, the heating wire being connected to a power source; The cooling section includes a cooling pipe body and a silicone tube disposed on the wall of the cooling pipe body.

9. The apparatus for preparing 6N high-purity boron according to claim 8, characterized in that, The heating wire is a tantalum wire with a purity of 99.9%, a diameter of 1mm-2mm, and a length that is 1cm-2cm shorter than the length of the reduction reaction section.

10. The apparatus for preparing 6N high-purity boron according to claim 8, characterized in that, The reduction reaction mechanism is made of silicon dioxide.

11. A method for preparing 6N high-purity boron, applied in the apparatus for preparing 6N high-purity boron as described in any one of claims 8-10, characterized in that, Includes the following steps: S100: Activate the cooling assembly of the Dewar canister to bring the outer surface temperature of the Dewar canister to a first preset temperature; S200: Turn on the first switch of the preheating section in the reduction reaction mechanism so that the temperature of the preheating section reaches the second preset temperature. When the temperature of the preheating section reaches the second preset temperature, turn on the second switch of the reduction reaction section in the reduction reaction mechanism so that the temperature of the preheating section reaches the third preset temperature, and keep the voltage constant. S300: The rate regulator is activated to deliver boron tribromide to the preheating section of the reduction reaction mechanism. At the same time, the hydrogen valve is opened, allowing the hydrogen in the hydrogen delivery mechanism to enter the preheating section of the reduction reaction mechanism and mix with the boron tribromide to form a mixed gas. The mixed gas enters the reduction reaction section of the reduction reaction mechanism to generate 6N high-purity boron. The unreacted boron tribromide enters the cooling section of the reduction reaction mechanism for cooling. S400: Turn off the cooling components of the Dewar canister, turn off the heating switch of the preheating section and the first switch of the reaction section in the reduction reaction mechanism, continue to introduce hydrogen for a preset time, and observe whether the sponge palladium detection mechanism expands. When the sponge palladium detection mechanism does not expand, open the argon valve and close the hydrogen valve until the room temperature is reached in the reduction reaction mechanism, then close the argon valve. S500: Collect the 6N high-purity boron.

12. The method for preparing 6N high-purity boron according to claim 11, characterized in that, Before step S100, the method further includes: checking the apparatus for preparing 6N high-purity boron for leaks; if the test is qualified, checking whether the silicone tube in the cooling zone of the reduction reaction mechanism is attached to the cooling zone.

13. The method for preparing 6N high-purity boron according to claim 11, characterized in that, The first preset temperature is 25℃-30℃, the second preset temperature is 95℃-100℃, and the third preset temperature is 1200℃-1300℃.

14. The method for preparing 6N high-purity boron according to claim 11, characterized in that, Step S500 specifically includes: S501: Wrap the heating wire and the 6N high-purity boron attached to the heating wire in a dust-free bag, and separate the heating wire and the 6N high-purity boron from the reduction reaction section using an ultrasonic cutter. S502: Break the 6N high-purity boron attached to the heating wire and separate the 6N high-purity boron from the heating wire.

15. The method for preparing 6N high-purity boron according to claim 14, characterized in that, The method also includes step S600, in which the density of the product of the divided 6N high-purity boron and the heating wire is measured by the water displacement method to determine the purity of the 6N high-purity boron.

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