CN114408880A - Method for preparing hexagonal boron nitride nanoparticles - Google Patents
Method for preparing hexagonal boron nitride nanoparticles Download PDFInfo
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- CN114408880A CN114408880A CN202210148766.9A CN202210148766A CN114408880A CN 114408880 A CN114408880 A CN 114408880A CN 202210148766 A CN202210148766 A CN 202210148766A CN 114408880 A CN114408880 A CN 114408880A
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- C01B21/00—Nitrogen; Compounds thereof
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Abstract
The invention relates to a method for preparing hexagonal boron nitride nanoparticles, which comprises the steps of taking boric acid and melamine as raw materials and carbon nanotubes as templates, preparing a boron nitride precursor by adopting a microwave method in intelligent full-automatic ultrasonic and microwave integrated equipment, and carrying out heat treatment on the boron nitride precursor in the intelligent full-automatic ultrasonic and microwave integrated equipment to prepare the boron nitride nanoparticles. The invention has the advantages of simple and convenient process, high automation degree and labor load saving.
Description
Technical Field
The invention belongs to the technical field of boron nitride nanoparticle preparation, and particularly relates to a method for preparing hexagonal boron nitride nanoparticles.
Background
Boron nitride is an inorganic ceramic material consisting of B atoms and N atoms, and is an artificially synthesized functional material with wide application and great development potential. The boron nitride has the characteristics of good heat resistance, acid corrosion resistance, high heat conduction, electric insulation, low thermal expansion coefficient, oxidation resistance and the like, so that the h-BN material has wide application in the fields of ceramics, metallurgy, coating paint, adsorption, catalysis and the like.
There are also many methods for synthesizing h-BN, such as: the traditional high temperature method, CVD method, solvothermal method, precursor method, template method, molten salt method and the like have advantages and disadvantages. For example, the hydrothermal method has mild synthesis conditions, easy control, simple process, few sample defects, uniform granularity, low yield and purity, unstable most of raw materials and solvents used for reaction, high toxicity and the like; the sample synthesized by the CVD method has uniform size, smooth appearance and higher purity, but has the problems of high requirement on synthesis equipment, troublesome substrate pretreatment, complex process, low yield, difficult accurate control of process parameters and the like. The preparation cost of the hexagonal boron nitride nano particles synthesized in the current market is very high, and the application of the hexagonal boron nitride nano particles is greatly restricted. Therefore, new processes and product-controlled synthesis methods are needed for the production of hexagonal boron nitride nanoparticles.
The micro-nano hexagonal boron nitride particles can be prepared by adopting an organic matter precursor method, namely, melamine and boric acid are adopted as raw materials, a carbon nano tube is adopted as a template, a rod-shaped precursor is synthesized by a wet chemical method, and then the boron nitride nanoparticles are obtained by heat treatment. The method for preparing hexagonal boron nitride has the advantages of low production cost and simple process flow.
In the process of preparing the hexagonal boron nitride nanoparticles, ultrasonic waves are required to be applied for dispersing and microwave heating to accelerate reaction, the existing preparation process is independently carried out in each link, the preparation of the hexagonal boron nitride nanoparticles needs to be manually operated, and full-automatic preparation cannot be well achieved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for preparing hexagonal boron nitride nano particles, which has the advantages of simple process, simple and convenient operation and high automation degree.
The technical scheme of the invention is as follows:
a method for preparing hexagonal boron nitride nanoparticles comprises the steps of taking boric acid and melamine as raw materials and carbon nanotubes as templates, preparing a boron nitride precursor by a microwave method in intelligent full-automatic ultrasonic and microwave integrated equipment, and carrying out heat treatment on the boron nitride precursor in the intelligent full-automatic ultrasonic and microwave integrated equipment to obtain the boron nitride nanoparticles;
the preparation process of the boron nitride precursor comprises the steps of adding carbon nano tubes into a beaker filled with 200 plus 500ml of deionized water in the intelligent full-automatic ultrasonic and microwave integrated equipment, applying ultrasonic waves for 2-4 hours for ultrasonic dispersion, adding boric acid and melamine after the ultrasonic waves are stopped, then applying microwaves, transferring the mixed liquid into a non-metal container, adding an ice-water mixture into the non-metal container, repeatedly washing and filtering the mixed liquid in the non-metal container by using deionized water and absolute ethyl alcohol after the mixed liquid is cooled, and finally applying microwaves to a filtered oversize product obtained by filtering for drying to obtain the boron nitride precursor;
the preparation process of the boron nitride nanoparticles comprises the steps of putting the boron nitride precursor into a crucible in the intelligent full-automatic ultrasonic microwave integrated equipment, carrying out heat treatment on the boron nitride precursor at the temperature of 1000-plus-one and 1400 ℃ for 3-6h in the nitrogen atmosphere, then cooling to the temperature of 600-plus-one and 900 ℃, adjusting to be an air atmosphere, carrying out heat preservation at the temperature of 600-plus-one and 900 ℃ for 1-6h, and removing the carbon nanotubes to obtain the boron nitride nanoparticles with the hole structures.
Further, the addition amount of the carbon nano tube is 1-10% of the mass of the expected synthesized boron nitride.
Further, the drying temperature of the filtered oversize is 30-60 ℃, and the drying time is 10-18 h.
Further, the molar ratio of melamine to boric acid is (0.25-4): 1.
further, the intelligent full-automatic ultrasonic and microwave integrated equipment comprises a working box with one side surface capable of being opened, an ultrasonic and microwave integrated machine, a multi-degree-of-freedom mechanical arm positioned at one side of the ultrasonic and microwave integrated machine, a storage table, a collecting box, a weighing table, a plurality of gas cylinders and a tubular heating furnace are arranged in the working box, the ultrasonic and microwave integrated machine comprises a microwave box which is erected in the working box and has one side surface capable of being opened, a plurality of magnetrons are installed on the microwave box, a temperature measuring hole for temperature monitoring through an infrared thermometer is formed in the top of the microwave box, an aluminum oxide ceramic amplitude transformer extending into the microwave box is installed at the bottom of the microwave box, an ultrasonic transducer is arranged at the lower end of the aluminum oxide ceramic amplitude transformer, an aluminum oxide ceramic placing seat for placing a beaker or a crucible is arranged at one end of the aluminum oxide ceramic amplitude transformer positioned in the microwave box, the aluminum oxide ceramic placing seat is provided with a jacking component for fixing a beaker or a crucible, the ultrasonic transducer is connected with an ultrasonic generator, the tubular heating furnace is provided with a plurality of air inlet pipes and an air outlet pipe, the air inlet pipes and the air outlet pipe are both provided with electromagnetic valves, the outer side of the working box is provided with a controller, and the controller is connected with the multi-degree-of-freedom mechanical arm, the magnetron, the electromagnetic valves, the infrared thermometer and the tubular heating furnace.
Further, the multi-degree-of-freedom mechanical arm is rotatably installed on the inner bottom surface of the working box, a clamping arm is arranged at the end part of the multi-degree-of-freedom mechanical arm, and the clamping arm can move in multiple dimensions under the driving of the multi-degree-of-freedom mechanical arm so as to clamp the beaker or the crucible to any preset working area.
Furthermore, a placing groove is formed in the top end of the alumina ceramic placing seat, the alumina ceramic placing seat is provided with a hollow inner cavity, the jacking component is partially assembled in the hollow inner cavity, the jacking component comprises an arc-shaped plate and an ejector rod connected to the arc-shaped plate, a baffle is arranged at the end of the ejector rod, a sleeve is arranged on one side wall of the hollow inner cavity, the ejector rod is arranged in the sleeve in a penetrating mode, an inner convex ring is arranged on the end wall of the sleeve, a spring is arranged in the sleeve, two ends of the spring are abutted to the side face of the hollow inner cavity and the baffle respectively, and a through hole matched with the arc-shaped plate is formed in the side wall of the placing groove so that the arc-shaped plate can move together with the ejector rod through the through hole.
Further, the object placing table is arranged on one side of the multi-freedom-degree mechanical arm according to preset requirements, the object placing table comprises a beaker, a crucible, a non-metal container and a filter screen which are placed according to the preset requirements, and the multi-freedom-degree mechanical arm can take and place the beaker or the crucible or the filter screen at a preset position according to control signals of the controller.
Further, the weighing platform is arranged on one side of the multi-degree-of-freedom mechanical arm according to a preset requirement, the weighing platform is provided with a carbon nano tube storage barrel, a deionized water storage barrel, a boric acid storage barrel, a melamine storage barrel, an absolute ethyl alcohol storage barrel and an ice water mixture storage barrel according to preset positions, discharge ports of the carbon nano tube storage barrel and the melamine storage barrel are respectively provided with a metering scale, discharge ports of the deionized water storage barrel, the boric acid storage barrel and the absolute ethyl alcohol storage barrel are respectively provided with a metering pump, and the multi-degree-of-freedom mechanical arm can be used for receiving the carbon nano tube, the deionized water, the boric acid, the melamine, the absolute ethyl alcohol or the ice water mixture at the preset positions according to control signals of the controller.
Furthermore, the two gas cylinders are respectively filled with nitrogen and air and are respectively connected to an electromagnetic valve of an air inlet pipe arranged at the lower part of the microwave box through an air path.
Compared with the prior art, the invention has the beneficial effects that:
1. firstly, preparing a boron nitride precursor coated with a carbon nano tube, and removing the carbon nano tube through heat treatment to obtain a boron nitride fiber material with a hole-containing structure; therefore, the method for preparing the hexagonal boron nitride has low cost, simple technical process and easy mass production;
2. in the process of preparing the boron nitride precursor and the boron nitride nanoparticles, the preparation is completed in the intelligent full-automatic ultrasonic and microwave integrated equipment, no personnel is required to perform specific operation in the whole preparation process, the addition of each raw material and the operation of the whole preparation process can be completed in the intelligent full-automatic ultrasonic and microwave integrated equipment, and the burden of the personnel is greatly reduced;
in a word, the invention has the advantages of simple and convenient process, high automation degree and labor load saving.
Drawings
FIG. 1 is a schematic structural view of the present invention;
fig. 2 is a partially enlarged view of a portion a in fig. 1.
In the figure, the device comprises a working box 1, a working box 2, a multi-degree-of-freedom mechanical arm 3, a storage table 4, a collecting box 5, a weighing table 6, an air bottle 7, a microwave box 8, a magnetron 9, an air inlet pipe 10, an air outlet pipe 11, an electromagnetic valve 12, a temperature measuring hole 13, an ultrasonic transducer 14, an alumina ceramic placing seat 15, an ultrasonic generator 16, a controller 17, a clamping arm 18, a placing groove 19, a hollow inner cavity 20, an arc-shaped plate 21, an ejector rod 22, a baffle plate 23, a sleeve barrel 24, an inner convex ring 25, a spring 26, an alumina ceramic amplitude-changing rod 27 and a tubular heating furnace.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for preparing hexagonal boron nitride nanoparticles comprises the steps of taking carbon nanotubes, boric acid and melamine as raw materials, preparing a boron nitride precursor by microwave irradiation in intelligent full-automatic ultrasonic and microwave integrated equipment, and carrying out heat treatment on the boron nitride precursor in the intelligent full-automatic ultrasonic and microwave integrated equipment to obtain the boron nitride nanoparticles;
the preparation process of the boron nitride precursor comprises the steps of adding a carbon nano tube into a beaker filled with 200 plus 500ml of deionized water in the intelligent full-automatic ultrasonic and microwave integrated equipment, applying ultrasonic waves for 2-4 hours for ultrasonic dispersion, adding boric acid and melamine after the ultrasonic application is stopped, then applying microwaves to keep the temperature at 90-100 ℃ for 40-60min, then transferring the mixed solution into a non-metal container, adding an ice water mixture into the non-metal container, repeatedly washing and filtering the mixed solution in the non-metal container by using deionized water and absolute ethyl alcohol after the mixed solution in the beaker is cooled, and finally applying microwaves to a filtered oversize product obtained by filtering for drying to obtain the boron nitride precursor;
the preparation process of the boron nitride nanoparticles comprises the steps of putting the boron nitride precursor into a crucible in the intelligent full-automatic ultrasonic microwave integrated equipment, carrying out heat treatment on the boron nitride precursor at the temperature of 1000-1400 ℃ for 3-6h under the nitrogen atmosphere, cooling to the temperature of 600-900 ℃, adjusting to be an air atmosphere, carrying out heat preservation at the temperature of 600-900 ℃ for 1-6h, and removing the carbon nanotubes to obtain the boron nitride nanoparticles with the pore structures.
In this embodiment, the addition amount of the carbon nanotubes is 1% to 10% of the mass of the expected synthesized boron nitride.
In the embodiment, the drying temperature of the filtered oversize material is 30-60 ℃, and the drying time is 10-18 h.
In this example, the molar ratio of melamine to boric acid was (0.25-4): 1.
as shown in fig. 1, the intelligent full-automatic ultrasonic and microwave integrated equipment comprises a work box 1 with one side surface being provided with an openable door, an ultrasonic and microwave integrated machine, a multi-degree-of-freedom mechanical arm 2 positioned at one side of the ultrasonic and microwave integrated machine, a storage table 3, a collection box 4, a weighing table 5, a plurality of gas cylinders 6 and a tubular heating furnace 27 are arranged in the work box 1, the ultrasonic and microwave integrated machine comprises a microwave box 7 which is erected in the work box 1 and has one side surface being provided with an openable door, a plurality of magnetrons 8 are arranged on the microwave box 7, a temperature measuring hole 12 for monitoring temperature through an infrared thermometer is arranged at the top of the microwave box 7, an alumina ceramic amplitude transformer 26 extending into the microwave box 7 is arranged at the bottom of the microwave box 7, an ultrasonic transducer 13 is arranged at the lower end of the alumina ceramic amplitude transformer 26 positioned in the microwave box 7, an alumina ceramic seat 14 for placing a beaker or a crucible is arranged at one end of the alumina ceramic amplitude transformer 26 positioned in the microwave box 7, the aluminum oxide ceramic placing seat 14 is provided with a jacking component for fixing a beaker or a crucible, the ultrasonic transducer 13 is connected with an ultrasonic generator 15, the tubular heating furnace 27 is provided with a plurality of air inlet pipes 9 and an air outlet pipe 10, the air inlet pipes 9 and the air outlet pipe 10 are both provided with electromagnetic valves 11, the outer side of the working box 1 is provided with a controller 16, and the controller 16 is connected with the multi-degree-of-freedom mechanical arm 2, the magnetron 8, the electromagnetic valves 11, the infrared thermometer and the tubular heating furnace 27.
In this embodiment, the multi-degree-of-freedom mechanical arm 2 is rotatably mounted on the inner bottom surface of the work box 1, a clamping arm 17 is provided at an end of the multi-degree-of-freedom mechanical arm 2, and the clamping arm 17 can move in multiple dimensions under the driving of the multi-degree-of-freedom mechanical arm 2, so as to clamp a beaker or a crucible to any preset work area.
As shown in fig. 2, a placing groove 18 is provided at the top end of the alumina ceramic placing seat 14, the alumina ceramic placing seat 14 has a hollow inner cavity 19, the tightening component is partially assembled in the hollow inner cavity 19, the tightening component includes an arc plate 20 and a mandrel 21 connected to the arc plate 20, a baffle 22 is provided at the end of the mandrel 21, a sleeve 23 is provided on one side wall of the hollow inner cavity 19, the mandrel 21 is inserted into the sleeve 23, an inner collar 24 is provided on the end wall of the sleeve 23, a spring 25 is provided in the sleeve 23, two ends of the spring 25 respectively abut against the side surface of the hollow inner cavity 19 and the baffle 22, a through hole adapted to the arc plate 20 is provided on the side wall of the placing groove 18, so that the arc plate 20 and the mandrel 21 can move through the through hole;
the sleeve 23 has a certain distance with one side wall of the hollow inner cavity 19, the side face of the arc plate 20 is provided with a top block, the top block can abut against the sleeve 23, under the elastic action of the spring 25, the ejector rod 21 has a tendency of moving towards the inside of the placing groove 18 to push the arc plate 20 to move towards the inside of the placing groove 18, so that a beaker or a crucible placed in the placing groove 18 is clamped and fixed, when the beaker or the crucible is taken away, the baffle plate 22 moves to the left end and the right end under the action of the spring 25, and the baffle plate 22 abuts against the inner convex ring 24.
In this embodiment, the object placing table 3 is disposed on one side of the multi-degree-of-freedom mechanical arm 2 according to a preset requirement, the object placing table 3 includes a beaker, a crucible, a non-metallic container and a filter screen which are disposed according to the preset requirement, and the multi-degree-of-freedom mechanical arm 2 can take and place the beaker, the crucible or the filter screen at a preset position according to a control signal of the controller 16.
In this embodiment, the weighing platform 5 is disposed on one side of the multi-degree-of-freedom mechanical arm 2 according to a preset requirement, the weighing platform 5 is provided with a carbon nanotube storage barrel, a deionized water storage barrel, a boric acid storage barrel, a melamine storage barrel, an absolute ethyl alcohol storage barrel, and an ice water mixture storage barrel according to preset positions, discharge ports of the carbon nanotube storage barrel and the melamine storage barrel are respectively provided with a metering scale, discharge ports of the deionized water storage barrel, the boric acid storage barrel, and the absolute ethyl alcohol storage barrel are respectively provided with a metering pump, the multi-degree-of-freedom mechanical arm 2 can be connected with the carbon nanotube, the deionized water, the boric acid, the melamine, the absolute ethyl alcohol, or the ice water mixture at the preset positions according to a control signal of the controller 16, and the metering scales and the metering pumps are both in signal connection with the controller 16.
In this embodiment, the number of the gas cylinders 6 is two, the two gas cylinders 6 are respectively filled with nitrogen and air, and the two gas cylinders 6 are respectively connected to the electromagnetic valve 11 of the gas inlet pipe 9 arranged at the lower part of the microwave box 7 through gas paths.
In this embodiment, a single chip microcomputer is disposed in the controller 16, a touch screen and a keyboard connected to the single chip microcomputer are disposed on the controller 16, a preset process for preparing the hexagonal boron nitride nanoparticles is integrated in the single chip microcomputer 16, and the single chip microcomputer 16 automatically calculates required raw materials and auxiliary materials in a production process according to the conditions of finished products of the hexagonal boron nitride nanoparticles to be configured.
In the process of preparing the boron nitride precursor, the multi-degree-of-freedom mechanical arm 2 clamps a beaker at a preset position of the beaker on a placing table 3 at the preset position through a clamping arm 17, the multi-degree-of-freedom mechanical arm 2 drives the clamping arm 17 to drive the beaker to the preset position of a deionized water storage barrel to receive deionized water, in the process of receiving the deionized water, a metering pump meters water yield, the metering pump stops working after reaching the preset water yield, the multi-degree-of-freedom mechanical arm 2 drives the clamping arm 17 to drive the beaker to the preset position of the carbon nanotube storage barrel to receive carbon nanotubes, a corresponding amount of carbon nanotubes are weighed by a meter discharged from the carbon nanotube storage barrel and put into the beaker, then the multi-degree-of-freedom mechanical arm 2 drives the clamping arm 17 to drive the beaker to a microwave box 7, the beaker is placed in a placing groove 18, and then the multi-degree-of freedom mechanical arm 2 exits the microwave box 7, the microwave box 7 is closed, the ultrasonic generator 15 is started, ultrasonic waves are applied to a mixture in the beaker, after the ultrasonic waves are applied, the ultrasonic waves are stopped being applied, the microwave box 7 is opened, the multi-degree-of-freedom mechanical arm 2 drives the clamping arm 17 to enter the microwave box 7 to clamp the beaker to a preset position of boric acid and melamine in sequence to take the boric acid and the melamine, the beaker is placed in the placing groove 18 again, after the microwave box 7 is closed, the magnetron 8 is started to heat the microwave box, after the heating is finished, the multi-degree-of-freedom mechanical arm 2 drives the clamping arm 17 to move the beaker to the placing table 3 again, mixed liquid in the beaker is poured into a non-metal container, then the multi-degree-of freedom mechanical arm 2 drives the non-metal container to the ice-water mixture, ice-water mixture is added into the non-metal container to be rapidly cooled, after cooling, the multi-degree-of-freedom mechanical arm 2 drives the clamping arm 17 to clamp the beaker to sequentially go to preset positions of deionized water and absolute ethyl alcohol to receive the deionized water and the absolute ethyl alcohol for washing, then the multi-degree-of-freedom mechanical arm 2 drives the clamping arm 17 to clamp the beaker to reach the preset position of the filter sieve for filtering, after the washing and the filtering are repeated for preset times, the multi-degree-of-freedom mechanical arm 2 drives the clamping arm 17 to clamp the beaker to return to the placing groove 18 again, and microwave is applied again for drying to obtain a boron nitride precursor; during the washing and filtering process, the filtered lower layer is discharged into a collecting barrel;
in the process of preparing the boron nitride nanoparticles, the multi-degree-of-freedom mechanical arm 2 drives the clamping arm 17 to clamp the beaker to a preset position of the crucible, and a boron nitride precursor is introduced into the crucible, then the multi-degree-of-freedom mechanical arm 2 drives the clamping arm 17 to clamp the crucible into the tubular heating furnace 27, after the multi-degree-of-freedom mechanical arm 2 drives the clamping arm 17 to exit from the tubular heating furnace 27, the door of the tubular heating furnace 27 is closed, the electromagnetic valve 11 of the nitrogen inlet pipe 9 is opened, the electromagnetic valve 11 of the air outlet pipe 10 is opened, after the preset time is reached, the electromagnetic valve 11 of the nitrogen inlet pipe 9 and the electromagnetic valve 11 of the air outlet pipe 10 are both closed, the tubular heating furnace 27 is opened again, the temperature is raised to any temperature in the middle of 1000-1400 ℃, the heat preservation time is any time within 3-6 hours, the controller 16 opens the door of the tubular heating furnace 27 and opens the door of the tubular heating furnace 27, after the temperature in the tubular heating furnace 27 is reduced to 600-.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (10)
1. A method of hexagonal boron nitride nanoparticles, characterized by: boric acid and melamine are used as raw materials, a carbon nano tube is used as a template, a boron nitride precursor is prepared by a microwave method in intelligent full-automatic ultrasonic and microwave integrated equipment, and the boron nitride precursor is subjected to heat treatment in the equipment to prepare the boron nitride nano particles.
The preparation process of the boron nitride precursor comprises the steps of adding a carbon nano tube into a beaker filled with 200 plus 500ml of deionized water in the intelligent full-automatic ultrasonic and microwave integrated equipment, applying ultrasonic waves for 2-4h for ultrasonic dispersion, adding boric acid and melamine, performing microwave heating to keep the temperature at 90-100 ℃ for 40-60min, transferring the mixed solution into a non-metal container, adding an ice water mixture into the non-metal container, repeatedly washing and filtering the mixed solution in the non-metal container by using deionized water and absolute ethyl alcohol after the mixed solution is cooled, and finally applying microwaves to filtered oversize products obtained by filtering for drying to obtain the boron nitride precursor;
the preparation process of the boron nitride nanoparticles comprises the steps of putting the boron nitride precursor into a crucible in the intelligent full-automatic ultrasonic microwave integrated equipment, carrying out heat treatment on the boron nitride precursor at the temperature of 1000-1400 ℃ for 3-6h under the nitrogen atmosphere, cooling to the temperature of 600-900 ℃, adjusting to be an air atmosphere, carrying out heat preservation at the temperature of 600-900 ℃ for 1-6h, and removing the carbon nanotubes to obtain the boron nitride nanoparticles with the pore structures.
2. The method of hexagonal boron nitride nanoparticles of claim 1, wherein: the addition amount of the carbon nano tube is 1-10% of the mass of the expected synthesized boron nitride.
3. The method of hexagonal boron nitride nanoparticles of claim 1, wherein: the drying temperature of the filtered oversize is 30-60 ℃, and the drying time is 10-18 h.
4. The method of hexagonal boron nitride nanoparticles of claim 1, wherein: the molar ratio of the melamine to the boric acid is as follows: 1.
5. the method of hexagonal boron nitride nanoparticles of claim 1, wherein: the intelligent full-automatic ultrasonic and microwave integrated equipment comprises a working box with one side surface capable of being opened, wherein an ultrasonic and microwave integrated machine, a multi-degree-of-freedom mechanical arm positioned on one side of the ultrasonic and microwave integrated machine, a storage table, a collecting box, a weighing table, a plurality of gas cylinders and a tubular heating furnace are arranged in the working box, the ultrasonic and microwave integrated machine comprises a microwave box which is erected in the working box and has one side surface capable of being opened, a plurality of magnetrons are arranged on the microwave box, the top of the microwave box is provided with a temperature measuring hole for temperature monitoring through an infrared thermometer, the bottom of the microwave box is provided with an alumina ceramic amplitude transformer extending into the microwave box, the lower end of the alumina ceramic amplitude transformer is provided with an ultrasonic transducer, one end of the alumina ceramic amplitude transformer positioned in the microwave box is provided with an alumina ceramic placing seat for placing a beaker or a crucible, the aluminum oxide ceramic placing seat is provided with a jacking component for fixing a beaker or a crucible, the ultrasonic transducer is connected with an ultrasonic generator, the tubular heating furnace is provided with a plurality of air inlet pipes and an air outlet pipe, the air inlet pipes and the air outlet pipe are both provided with electromagnetic valves, the outer side of the working box is provided with a controller, and the controller is connected with the multi-degree-of-freedom mechanical arm, the magnetron, the electromagnetic valves, the infrared thermometer and the tubular heating furnace.
6. The method of hexagonal boron nitride nanoparticles of claim 5, wherein: the multi-degree-of-freedom mechanical arm is rotatably arranged on the inner bottom surface of the working box, a clamping arm is arranged at the end part of the multi-degree-of-freedom mechanical arm, and the clamping arm can move in multiple dimensions under the driving of the multi-degree-of-freedom mechanical arm so as to clamp a beaker or a crucible to any preset working area.
7. The method of hexagonal boron nitride nanoparticles of claim 5, wherein: the top of the alumina ceramic placing seat is provided with a placing groove, the alumina ceramic placing seat is provided with a hollow inner cavity, the part of the jacking component is assembled in the hollow inner cavity, the jacking component comprises an arc-shaped plate and a push rod connected to the arc-shaped plate, the end part of the push rod is provided with a baffle, one side wall of the hollow inner cavity is provided with a sleeve, the push rod is arranged in the sleeve in a penetrating mode, the end wall of the sleeve is provided with an inner convex ring, a spring is arranged in the sleeve, two ends of the spring are respectively abutted to the side face of the hollow inner cavity and the baffle, and the side wall of the placing groove is provided with a through hole matched with the arc-shaped plate, so that the arc-shaped plate can move together with the push rod through the through hole.
8. The method of hexagonal boron nitride nanoparticles of claim 5, wherein: the object placing table is arranged on one side of the multi-degree-of-freedom mechanical arm according to preset requirements, a beaker, a crucible, a non-metal container and a filter screen are placed on the object placing table according to the preset requirements, and the multi-degree-of-freedom mechanical arm can take and place the beaker or the crucible or the filter screen at a preset position according to control signals of a controller.
9. The method of hexagonal boron nitride nanoparticles of claim 5, wherein: the device comprises a weighing platform, a carbon nanotube storage barrel, a deionized water storage barrel, a boric acid storage barrel, a melamine storage barrel, an absolute ethyl alcohol storage barrel and an ice water mixture storage barrel, wherein the weighing platform is arranged on one side of the multi-degree-of-freedom mechanical arm according to a preset requirement, the weighing platform is provided with the carbon nanotube storage barrel, the deionized water storage barrel, the boric acid storage barrel, the melamine storage barrel, the absolute ethyl alcohol storage barrel and the ice water mixture storage barrel according to preset positions, discharge ports of the carbon nanotube storage barrel and the melamine storage barrel are respectively provided with a metering pump, and the multi-degree-of-freedom mechanical arm can be connected with the carbon nanotube, the deionized water, the boric acid, the melamine, the absolute ethyl alcohol or the ice water mixture at the preset positions according to control signals of a controller.
10. The method of hexagonal boron nitride nanoparticles of claim 5, wherein: the microwave oven is characterized in that the number of the gas cylinders is two, the two gas cylinders are respectively filled with nitrogen and air, and the two gas cylinders are respectively connected to an electromagnetic valve of a gas inlet pipe arranged at the lower part of the microwave oven through a gas circuit.
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| CN104729294A (en) * | 2015-03-20 | 2015-06-24 | 重庆科技学院 | Ultrasonic vibration activation assisted microwave sintering furnace |
| CN207906265U (en) * | 2018-03-09 | 2018-09-25 | 宝鸡文理学院 | A kind of novel aluminum oxide ceramic fastener |
| CN109706550A (en) * | 2019-01-14 | 2019-05-03 | 中原工学院 | A kind of method that carbon nano-fiber prepares hexagonal boron nitride as template |
| US20210401522A1 (en) * | 2020-06-26 | 2021-12-30 | Procept Biorobotics Corporation | Integration of robotic arms with surgical probes |
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