CN111168076A - Preparation system and preparation method for nano conductor or semiconductor material with controllable size - Google Patents
Preparation system and preparation method for nano conductor or semiconductor material with controllable size Download PDFInfo
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Abstract
The invention discloses a preparation system and a preparation method of nano-conductor or semiconductor materials with controllable size, which comprises a nano-material preparation device, a size control device and a collection device which are sequentially communicated, wherein the nano-material preparation device consists of a power supply, an electrode, an ablation reaction container and an inert gas source, the size control device is a tubular furnace for carrying out heat treatment on the nano-conductor or semiconductor materials, and the collection device comprises a collection box; two electrode fixing seats used for installing and fixing electrodes are arranged in the ablation reaction container, the two electrode fixing seats are oppositely arranged on the inner wall of the ablation reaction container, and the two electrode fixing seats are respectively and electrically connected with two poles of a power supply. The final size of the nano conductor or semiconductor material is controlled by adjusting the temperature in the tubular furnace, the length of the tubular furnace and the speed of the nano conductor or semiconductor material along with the inert gas through the tubular furnace in the size control device, thereby changing the heat treatment temperature and the heat treatment time of the nano conductor or semiconductor material in the tubular furnace.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a preparation system and a preparation method with controllable size of a nano conductor or semiconductor material.
Background
The nano conductor or semiconductor material shows different physical and chemical properties from macroscopic block materials due to the basic characteristics of small-size effect, surface interface effect, quantum size effect and the like, and has huge application prospects in the fields of electronics, catalysis, lubrication, antibiosis, biomedicine and the like. Especially, the preparation of nano-conductor or semiconductor materials with different sizes has been receiving extensive attention, because the nano-conductor or semiconductor materials with different sizes have significant difference in material properties, and have great influence on the optical, electrical, magnetic and catalytic properties of devices. The requirements of high performance and low cost can be met only by matching nano conductors or semiconductor materials with different sizes on different occasions, for example, in the field of photocatalysis, the photocatalytic activity of titanium dioxide depends on the size of the titanium dioxide to a great extent, and the preparation of titanium dioxide with controllable size is an effective way for improving the photocatalytic performance of titanium dioxide.
At present, there are two major categories of chemical methods and physical methods for controlling the size of the nano conductor or semiconductor material, wherein the chemical methods mostly control the size of the nano conductor or semiconductor material through liquid phase reaction, but the liquid phase reaction has difficulty in continuously controlling the whole reaction process because of a series of factors including the concentration of reactants, the reaction temperature, the reaction time, and the like. The physical principle is that nano conductor or semiconductor materials with different sizes are prepared by adding a proper precipitator into a sol-gel method, controlling the pH value of a system and the relative proportion of water or a surfactant in a microemulsion method and the like, but the size control is difficult to grasp, and the nano particles with uniform particle sizes are difficult to accurately obtain.
Disclosure of Invention
In view of the above-mentioned drawbacks, the present invention is directed to a system and a method for manufacturing a nano-conductor or semiconductor material with controllable dimensions.
In order to achieve the purpose, the invention adopts the following technical scheme: the preparation system with the controllable size of the nano conductor or the semiconductor material comprises a nano material preparation device, a size control device and a collection device which are sequentially communicated, wherein the nano material preparation device consists of a power supply, an electrode, an ablation reaction container and an inert gas source, the size control device is a tubular furnace for carrying out heat treatment on the nano conductor or the semiconductor material, the collection device comprises a collection box, the inert gas source is communicated with the ablation reaction container, the ablation reaction container is communicated with the tubular furnace, the tubular furnace is communicated with the collection box, and the bottom of the collection box is provided with an exhaust hole; two electrode fixing seats for installing and fixing the electrodes are arranged in the ablation reaction container, the two electrode fixing seats are oppositely arranged on the inner wall of the ablation reaction container, and the two electrode fixing seats are respectively and electrically connected with two poles of the power supply; the two-end electrodes are bulk materials of the components of the nano conductor or semiconductor material required to be prepared; and a bearing substrate for bearing and collecting the nano conductor or the semiconductor material is arranged in the collecting box.
Further, the tube furnace is any one of a single-temperature-zone tube furnace, a double-temperature-zone tube furnace and a multi-temperature-zone tube furnace.
Further, the ablation reaction container is provided with an air inlet pipeline and a first air outlet pipeline, the ablation reaction container is communicated to the inert gas source through the air inlet pipeline, the ablation reaction container is communicated to the tube furnace through the first air outlet pipeline, the tube furnace is provided with a second air outlet pipeline, the tube furnace is communicated to the collecting device through the second air outlet pipeline, and the air inlet pipeline, the first air outlet pipeline and the second air outlet pipeline are all provided with one-way valves for controlling the flow rate of inert gas.
Further, the ablation reaction vessel is a closed cuboid vessel, the two electrode fixing seats are oppositely arranged on the upper wall and the lower wall of the ablation reaction vessel respectively from top to bottom, the air inlet pipeline and the first air outlet pipeline are oppositely arranged on the left wall and the right wall of the ablation reaction vessel respectively from left to right, the mounting axes of the two electrode fixing seats are on the same vertical straight line, the mounting axes of the air inlet pipeline, the first air outlet pipeline and the second air outlet pipeline are all arranged on the same horizontal straight line, and the mounting axes of the electrode fixing seats and the mounting axis of the air inlet pipeline are intersected at the midpoint of the ablation reaction vessel.
Furthermore, the collecting device also comprises a vertically arranged deposition pipeline, the upper end of the deposition pipeline is communicated with the tail end of the second gas outlet pipeline, and the lower end of the deposition pipeline is arranged right above the bearing substrate.
Furthermore, the ablation reaction vessel is provided with a first threaded hole for installing the electrode fixing seat, the electrode fixing seat comprises a fixing round platform, an adjusting screw rod and an electrode base, the fixing round platform is provided with an external thread matched with the first threaded hole, the fixing round platform is provided with a second threaded hole matched with the adjusting screw rod at the central axis of the fixing round platform, and the electrode base is fixedly connected to the tail end of the adjusting screw rod.
Furthermore, the bottom end of the electrode base is provided with a conducting strip electrically connected with the power supply, and the side wall of the electrode base is provided with a plurality of locking screw rods used for clamping the electrodes.
The preparation method of the nano conductor or semiconductor material with controllable size is prepared by adopting the preparation system of the nano conductor or semiconductor material with controllable size, and comprises the following preparation steps:
s1: the two electrodes are respectively installed and fixed on the two electrode fixing seats, the two electrodes are adjusted to be in the same straight line, and the distance between the reaction end faces of the two electrodes is 0.1-3 mm;
s2: opening an inert gas source and adjusting the flow rate of the inert gas, and smoothly introducing the inert gas into the ablation reaction container for 3-5 mins;
s3: preheating the tube furnace to reach a preset temperature;
s4: switching on a power supply, carrying out high-voltage spark ablation reaction on electrodes at two ends to produce a nano conductor or semiconductor material, and simultaneously, feeding the produced nano conductor or semiconductor material into a tubular furnace along with inert gas flow for heat treatment;
s5: the heat-treated nano conductor or semiconductor material enters the collecting box along with the inert gas flow and is deposited on the bearing substrate.
Further, the temperature of the tubular furnace is 20-1500 ℃, the inner diameter of the tubular furnace is 1-500 mm, and the length of the tubular furnace is 0.1-2 m.
Further, the inert gas source is any one of nitrogen, argon and helium, and the flow rate of the inert gas is 0.1-20L/min.
According to the preparation system and the preparation method, the electrodes at two ends generate high-voltage spark ablation reaction to produce the nano conductor or semiconductor material, the nano conductor or semiconductor material is sent into the tubular furnace through inert gas flow to be subjected to heat treatment, and finally the nano conductor or semiconductor material enters the collecting box and is deposited on the receiving substrate.
By utilizing the low-melting-point characteristic of the nano conductor or semiconductor material, atoms on the surface of particles can be subjected to atomic diffusion at a lower temperature, so that the nano conductor or semiconductor material is sent into the tube furnace for heat treatment, and then the nano conductor or semiconductor material is fused together to form nano conductor or semiconductor materials with different sizes; the temperature in the tubular furnace, the length of the tubular furnace and the speed of the nano conductor or semiconductor material passing through the tubular furnace along with the inert gas in the size control device are adjusted, so that the heat treatment temperature and the heat treatment time of the nano conductor or semiconductor material in the tubular furnace are changed, the final size of the nano conductor or semiconductor material is controlled, the purpose of controlling the size of the nano conductor or semiconductor material is achieved, the processing technology is quicker, simpler and environment-friendly, and the production cost is reduced. The heat treatment can be regulated and controlled in the production process, the size controllable accuracy of the nano conductor or semiconductor material is ensured, the particle size of the nano conductor or semiconductor material is more concentrated, the monodispersity is good, the processing process is stable and controllable, and the method is suitable for industrial production;
carrying nano conductor or semiconductor materials through inert gas flow, combining the nano material preparation device, the size control device and the collecting device into a continuous preparation system through flowing inert gas, reducing the transfer of the nano conductor or semiconductor materials, saving the steps of filtering, drying and the like, and then entering the tubular furnace for heat treatment, and being convenient to operate; and the nano conductor or semiconductor material particles leave the reaction end face of the electrode under the influence of inert gas flow, so that the phenomenon that local nano conductor or semiconductor materials stay in a reaction area for a long time to react continuously is avoided, and the preparation of nano conductor or semiconductor materials with concentrated particle sizes is facilitated; and inert gas is used as an environment for ablation reaction, so that the pollution of the nano conductor or semiconductor material caused by the active gas participating in the ablation reaction is reduced, and the purity of the nano conductor or semiconductor material is improved.
Drawings
FIG. 1 is a schematic structural diagram of a nano-conductor or semiconductor material fabrication system of the present invention;
FIG. 2 is a schematic diagram of the structure of an ablation reaction vessel in the nano-conductor or semiconductor material preparation system of the present invention;
FIG. 3 is a schematic diagram of the mechanism for fixing the circular truncated cone in the nano-conductor or semiconductor material preparation system according to the present invention;
FIG. 4 is a schematic structural diagram of an electrode holder in the nano-conductor or semiconductor material manufacturing system of the present invention.
Wherein: 1. a power source; 2. an electrode; 3. ablating the reaction vessel; 4. an inert gas source; 5. a tube furnace; 6. a collection box; 7. an exhaust hole; 8. an electrode holder; 9. receiving a substrate; 10. an air intake line; 11. a first gas outlet pipeline; 12. a second outlet pipeline; 13. a one-way valve; 14. a deposition pipeline; 15. a first threaded hole; 16. fixing the round table; 17. adjusting the screw rod; 18. an electrode base; 19. an external thread; 20. a second threaded hole; 21. a conductive sheet; 22. and locking the screw rod.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
As shown in fig. 1-4, the system for preparing nano conductor or semiconductor material with controllable size comprises a nano material preparation device, a size control device and a collection device which are sequentially communicated, wherein the nano material preparation device is composed of a power supply 1, an electrode 2, an ablation reaction container 3 and an inert gas source 4, the size control device is a tube furnace 5 for performing heat treatment on nano conductor or semiconductor material, the collection device comprises a collection box 6, the inert gas source 4 is communicated with the ablation reaction container 3, the ablation reaction container 3 is communicated with the tube furnace 5, the tube furnace 5 is communicated with the collection box 6, and the bottom of the collection box 6 is provided with an exhaust hole 7; two electrode fixing seats 8 for installing and fixing the electrodes 2 are arranged in the ablation reaction vessel 3, the two electrode fixing seats 8 are oppositely arranged on the inner wall of the ablation reaction vessel 3, and the two electrode fixing seats 8 are respectively and electrically connected with two poles of the power supply 1; the two-end electrodes 2 are block materials of the components of the nano conductor or semiconductor material required to be prepared; the collecting box 6 is internally provided with a bearing substrate 9 for bearing and collecting nano-conductor or semiconductor materials.
The working principle of the invention is as follows: after the power supply 1 is switched on, the electrodes 2 at two ends generate high-voltage spark ablation reaction to produce nano conductor or semiconductor materials, the nano conductor or semiconductor materials are sent into the tubular furnace 5 through inert gas flow for heat treatment, and finally the nano conductor or semiconductor materials enter the collecting box 6 and are deposited on the bearing substrate 9. By utilizing the low-melting-point characteristic of the nano conductor or semiconductor material, atoms on the surface of the particles can be subjected to atomic diffusion at a lower temperature, so that the nano conductor or semiconductor material is fed into the tube furnace 5 for heat treatment, and then the nano conductor or semiconductor material is fused together to form nano conductor or semiconductor materials with different sizes; the temperature in the tubular furnace 5, the length of the tubular furnace 5 and the speed of the nano conductor or semiconductor material passing through the tubular furnace 5 along with the inert gas in the size control device are adjusted, so that the heat treatment temperature and the heat treatment time of the nano conductor or semiconductor material in the tubular furnace 5 are changed, the final size of the nano conductor or semiconductor material is controlled, the purpose of controlling the size of the nano conductor or semiconductor material is achieved, the processing technology is quicker, simpler and environment-friendly, and the production cost is reduced. The method has the advantages of regulation and control in the production process, capability of ensuring the accuracy of size control of the nano conductor or semiconductor material, more centralized particle size of the nano conductor or semiconductor material, good monodispersity, stable and controllable processing process and suitability for industrial production.
The nano conductor or semiconductor material is carried by the inert gas flow, the nano material preparation device, the size control device and the collecting device are combined into a continuous preparation system by the flowing inert gas, the transfer of the nano conductor or semiconductor material is reduced, the steps of filtering, drying and the like are omitted, and the nano conductor or semiconductor material can enter the tubular furnace 5 for heat treatment, so that the operation is convenient; and the nano conductor or semiconductor material particles leave the reaction end face of the electrode 2 under the influence of inert gas flow, so that the phenomenon that local nano conductor or semiconductor materials stay in a reaction area for a long time to react continuously is avoided, and the preparation of nano conductor or semiconductor materials with concentrated particle sizes is facilitated; and inert gas is used as an environment for ablation reaction, so that the pollution of the nano conductor or semiconductor material caused by the active gas participating in the ablation reaction is reduced, and the purity of the nano conductor or semiconductor material is improved.
Specifically, the tube furnace 5 is any one of a single-temperature-zone tube furnace, a dual-temperature-zone tube furnace and a multi-temperature-zone tube furnace. Because different nano conductors or semiconductor materials have different heat treatment modes, different tube furnaces 5 are selected according to different prepared nano conductors or semiconductor materials, and the practicability of the preparation system is improved. The total length of the heat treatment temperature zone is shortened by reducing the number of the temperature zone works, and conversely, the total length of the heat treatment temperature zone is lengthened by increasing the number of the temperature zone works. The total length of the heat treatment temperature zone is rapidly changed by changing the number of the working temperature zones of the multi-temperature zone tube furnace, and the use is flexible.
Wherein: the ablation reaction container 3 is provided with an air inlet pipeline 10 and a first air outlet pipeline 11, the air inlet pipeline 10 is used for communicating the ablation reaction container 3 to the inert gas source 4, the first air outlet pipeline 11 is used for communicating the ablation reaction container 3 to the tube furnace 5, the tube furnace 5 is provided with a second air outlet pipeline 12, the second air outlet pipeline 12 is used for communicating the tube furnace 5 to the collecting device, and the air inlet pipeline 10, the first air outlet pipeline 11 and the second air outlet pipeline 12 are all provided with one-way valves 13 used for controlling the flow rate of the inert gas to be fast and slow. The air inlet pipeline 10, the first air outlet pipeline 11 and the second air outlet pipeline 12 are all provided with one-way valves 13, the flow rate of inert gas in each area is adjusted through the one-way valves 13, so that the time for the nano conductor or semiconductor material to pass through the tube furnace 5 can be estimated and adjusted, and the size of the nano conductor or semiconductor material can be accurately controlled.
Further, the ablation reaction vessel 3 is a closed cuboid vessel, the two electrode fixing seats 8 are oppositely arranged on the upper wall and the lower wall of the ablation reaction vessel 3 from top to bottom, the air inlet pipeline 10 and the first air outlet pipeline 11 are oppositely arranged on the left wall and the right wall of the ablation reaction vessel 3 from left to right, the mounting axes of the two electrode fixing seats 8 are on the same vertical straight line, the mounting axes of the air inlet pipeline 10, the first air outlet pipeline 11 and the second air outlet pipeline 12 are on the same horizontal straight line, and the mounting axis of the electrode fixing seat 8 and the mounting axis of the air inlet pipeline 10 are intersected at the midpoint of the ablation reaction vessel 3. Specifically, as shown in fig. 1, after the electrodes 2 are mounted on the electrode fixing seat 8, the ablation reaction of the two electrodes 2 is located on the path of the inert gas flow, which is beneficial to the inert gas flow to carry the nano-conductor or semiconductor material to enter the tube furnace 5 and the collecting device, and the ablation reaction of part of the nano-conductor or semiconductor material in the reaction area for a long time is avoided, which is beneficial to the production of the nano-conductor or semiconductor material with uniform size.
Further, the collecting device also comprises a deposition pipeline 14 which is vertically arranged, the upper end of the deposition pipeline 14 is communicated with the tail end of the second gas outlet pipeline 12, and the lower end of the deposition pipeline 14 is arranged right above the receiving substrate 9. Specifically, as shown in fig. 1, the nano conductor or semiconductor material is introduced into the collection box 6 through a vertically arranged deposition pipeline 14, so that the nano conductor or semiconductor material can be vertically deposited on the receiving substrate 9, and the collection effect is improved.
Further, as shown in fig. 2, the ablation reaction vessel 3 is provided with a first threaded hole 15 for mounting the electrode holder 8. As shown in fig. 4, the electrode holder 8 includes a fixing boss 16, an adjusting screw 17, and an electrode base 18. As shown in fig. 3, the fixing circular truncated cone 16 is provided with an external thread 19 for cooperating with the first threaded hole 15, the fixing circular truncated cone 16 is provided with a second threaded hole 20 at a central axis thereof for cooperating with the adjusting screw 17, and the electrode base 18 is fixedly connected to a distal end of the adjusting screw 17. The electrode fixing seat 8 is detachably fixed on the ablation reaction vessel 3 in a threaded connection mode, so that the electrode fixing seat 8 can be conveniently detached to replace the electrode 2; the electrode base 18 is fixedly connected to the tail end of the adjusting screw 17, so that the position of the electrode 2 can be changed by rotating the adjusting screw 17, and the distance between the two electrodes 2 can be conveniently adjusted.
Further, as shown in fig. 4, a bottom end of the electrode base 18 is provided with a conductive sheet 21 electrically connected to the power supply 1, and a side wall of the electrode base 18 is provided with a plurality of locking screws 22 for clamping the electrode 2. The electrodes 2 are clamped by the locking screws 22, and the electrodes 2 suitable for different diameters are fixedly arranged on the electrode base 18.
The size-controllable preparation method of the nano conductor or the semiconductor material is prepared by adopting the size-controllable preparation system of the nano conductor or the semiconductor material, and comprises the following preparation steps:
s1: the two electrodes 2 are respectively installed and fixed on the two electrode fixing seats 8, the two electrodes 2 are adjusted to be in the same straight line, and the distance between the reaction end faces of the two electrodes 2 is 0.1-3 mm;
s2: opening an inert gas source 4 and adjusting the flow rate of the inert gas, and smoothly introducing the inert gas into the ablation reaction container 3 for 3-5 mins; the method has the advantages of discharging fine impurities and active gas in the preparation of the preparation system with controllable size of the nano conductor or semiconductor material, avoiding the fine impurities and the active gas from participating in ablation reaction to pollute the nano conductor or semiconductor material, and improving the purity of the prepared nano conductor or semiconductor material
S3: preheating the tube furnace 5 to make the tube furnace 5 reach a preset temperature;
s4: switching on a power supply 1, introducing a voltage of 0.1-5 KV and a current of 1-20 mA to the electrodes 2 at the two ends, generating a high-voltage spark ablation reaction on the electrodes 2 at the two ends to generate a nano conductor or a semiconductor material, and simultaneously, feeding the generated nano conductor or semiconductor material into a tubular furnace 5 along with inert gas flow for heat treatment;
s5: the heat treated nano-conductor or semiconductor material follows the inert gas flow into the collection box 6 and is deposited on the receiving substrate 9.
The material of the electrode 2 may be any one of iron, aluminum, copper, zinc, titanium, aluminum, magnesium, potassium, sodium, calcium, strontium, barium, lead, tin, cobalt, nickel, antimony, mercury, cadmium, bismuth, gold, silver, platinum, ruthenium, rhodium, palladium, osmium, iridium, beryllium, lithium, rubidium, cesium, titanium, zirconium, vanadium, niobium, tantalum, tungsten, molybdenum, gallium, indium, thallium, germanium, rhenium, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium, yttrium, thorium, and other metal materials, or any one of silicon, germanium, selenium, gallium arsenide, silicon carbide, gallium nitride, cadmium sulfide, zinc sulfide, gallium phosphide, indium phosphide, cadmium, zinc telluride, lead sulfide, lead selenide and other semiconductor materials.
The receiving substrate 9 is a substrate which is favorable for deposition of a nano conductor or a semiconductor material, such as any one of semiconductor substrates of silicon, silicon carbide or gallium nitride, and may be one of organic thin film flexible substrates of PI, PET, fiberglass cloth, epoxy resin, acrylic resin or paper base, or any one of porous substrates of two-dimensional filter membrane, foamed nickel, foamed copper, foamed silver, foamed iron, foamed alloy, three-dimensional graphene foam, and the like.
Further, the temperature of the tubular furnace 5 is 20-1500 ℃, the inner diameter of the tubular furnace 5 is 1-500 mm, and the length of the tubular furnace 5 is 0.1-2 m. The larger the inner diameter of the tubular furnace 5 is, the more the nano materials of the nano conductor or the semiconductor material enter the tubular furnace per second for heat treatment are, so that the heat treatment efficiency is improved, but if the inner diameter of the tubular furnace 5 is too large, the concentration of the nano materials in the cavity of the tubular furnace 5 is low, and the fusion effect of the nano materials is reduced, so that the inner diameter of the tubular furnace 5 is 1-500 mm. The heat treatment temperature and the heat treatment time of the nano conductor or semiconductor material in the tubular furnace 5 are changed by adjusting the temperature in the tubular furnace 5, the entering amount of the nano conductor or semiconductor and the length of the tubular furnace 5 in the size control device, so that the final size of the nano conductor or semiconductor material is controlled, the purpose of controlling the size of the nano conductor or semiconductor material is achieved, the processing technology is quicker, simpler and environment-friendly, and the production cost is reduced. The method has the advantages of regulation and control in the production process, capability of ensuring the accuracy of size control of the nano conductor or semiconductor material, more centralized particle size of the nano conductor or semiconductor material, good monodispersity, stable and controllable processing process and suitability for industrial production.
Further, the inert gas source 4 is any one of nitrogen, argon and helium, and the flow rate of the inert gas is 0.1-20L/min. By changing the flow rate of the inert gas, the phenomenon that a local nano conductor or semiconductor material stays in a reaction area for a long time to continuously react is avoided, the nano conductor or semiconductor material with uniform size is produced, the time for the nano conductor or semiconductor material to pass through the tubular furnace 5 is changed, and the particle size of the nano conductor or semiconductor material is controlled. Wherein, the slower the inert gas flow rate, the longer the heat treatment time of the nano conductor or semiconductor material in the tube furnace 5, the larger the amount of change in the particle size of the nano conductor or semiconductor material, and conversely, the faster the inert gas flow rate, the shorter the heat treatment time of the nano conductor or semiconductor material, the smaller the amount of change in the particle size of the nano conductor or semiconductor material.
Specific examples of the nano conductor material or the nano semiconductor material manufactured according to the above-mentioned system and method for manufacturing a nano conductor or a semiconductor material with controllable size are shown in table 1:
TABLE 1
In table 1, the tube temperature of 200/800 ℃ means that the tube furnace 5 is a multi-temperature-zone tube furnace, the temperature of the temperature zone through which the nanoparticles pass first is 200 ℃, and the temperature of the temperature zone through which the nanoparticles pass later is 800 ℃.
As shown in table 1, in example 1, the temperature of the tube furnace 5 was 25 ℃ at normal temperature, and the nanomaterial having a particle size of 2 ± 1nm was produced at normal temperature. Comparing example 1 with example 2, it is clear that in example 2, when the temperature of the tube furnace 5 is 300 ℃, the nanoparticles are fused by heating in the tube furnace 5 due to the low melting point characteristic thereof, thereby producing the nanomaterial with the particle size of 8 ± 2 nm.
Comparing example 2 with example 3, it is clear that as the temperature of the tube furnace 5 is increased, the degree of fusion of the nanoparticles is increased, and the nanomaterial with larger particle size is produced.
As is clear from comparison between examples 3 and 6, the faster the nanoparticles are produced by increasing the reaction voltage and the reaction current of the electrodes 2 at both ends, and the nanoparticles can be produced with a large particle size due to a short ablation time.
Comparing example 4 with example 6, the two examples prepared nano materials with similar particle size, in example 4, the length of the heat treatment temperature zone is 1m, so that the heat treatment time of the nano materials in the tube furnace 5 is relatively longer, thereby improving the fusion degree of the nano conductor materials and producing the nano materials with large particle size. In example 6, the larger reaction voltage and reaction current are applied to the electrodes 2 at the two ends to reduce the ablation time of the nanoparticles, thereby preparing the nanomaterial with large particle size. Compared with the embodiment 6, the embodiment 4 can realize the enlargement of the particle size of the nano material only by lengthening the length of the heat treatment temperature zone, the operation is simple, the environment is protected, and the production cost is reduced.
As is clear from examples 7 to 12, the nanomaterial preparation system and the nanomaterial preparation method provided by the present invention are both suitable for the preparation of semiconductor materials, have good applicability, and are convenient for the preparation of different nanomaterials.
In the invention, the low melting point characteristic of the nano conductor or semiconductor material is utilized, atoms on the surface of the particles can be subjected to atomic diffusion at a lower temperature, so that the nano conductor or semiconductor material is fed into the tube furnace 5 for heat treatment, and is fused together to form nano conductor or semiconductor materials with different sizes; the temperature in the tubular furnace 5, the length of the tubular furnace 5 and the speed of the nano conductor or semiconductor material passing through the tubular furnace 5 along with the inert gas in the size control device are adjusted, so that the heat treatment temperature and the heat treatment time of the nano conductor or semiconductor material in the tubular furnace 5 are changed, the final size of the nano conductor or semiconductor material is controlled, the purpose of controlling the size of the nano conductor or semiconductor material is achieved, the processing technology is quicker, simpler and environment-friendly, and the production cost is reduced. The method has the advantages of regulation and control in the production process, capability of ensuring the accuracy of size control of the nano conductor or semiconductor material, more centralized particle size of the nano conductor or semiconductor material, good monodispersity, stable and controllable processing process and suitability for industrial production.
The nano conductor or semiconductor material is carried by the inert gas flow, the nano material preparation device, the size control device and the collecting device are combined into a continuous preparation system by the flowing inert gas, the transfer of the nano conductor or semiconductor material is reduced, the steps of filtering, drying and the like are omitted, and the nano conductor or semiconductor material can enter the tubular furnace 5 for heat treatment, so that the operation is convenient; and the nano conductor or semiconductor material particles leave the reaction end face of the electrode 2 under the influence of inert gas flow, so that the phenomenon that local nano conductor or semiconductor materials stay in a reaction area for a long time to react continuously is avoided, and the preparation of nano conductor or semiconductor materials with concentrated particle sizes is facilitated; and inert gas is used as an environment for ablation reaction, so that the pollution of the nano conductor or semiconductor material caused by the active gas participating in the ablation reaction is reduced, and the purity of the nano conductor or semiconductor material is improved.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive effort, which would fall within the scope of the present invention.
Claims (10)
1. The preparation system with controllable nano conductor or semiconductor material size is characterized in that: the device comprises a nano material preparation device, a size control device and a collection device which are sequentially communicated, wherein the nano material preparation device is composed of a power supply (1), an electrode (2), an ablation reaction container (3) and an inert gas source (4), the size control device is a tubular furnace (5) used for carrying out heat treatment on nano conductors or semiconductor materials, the collection device comprises a collection box (6), the inert gas source (4) is communicated with the ablation reaction container (3), the ablation reaction container (3) is communicated with the tubular furnace (5), the tubular furnace (5) is communicated with the collection box (6), and the bottom of the collection box (6) is provided with an exhaust hole (7); two electrode fixing seats (8) for installing and fixing the electrodes (2) are arranged in the ablation reaction container (3), the two electrode fixing seats (8) are oppositely arranged on the inner wall of the ablation reaction container (3), and the two electrode fixing seats (8) are respectively and electrically connected with two poles of the power supply (1); the two-end electrodes (2) are bulk materials of the components of the nano conductor or semiconductor material required to be prepared; the collecting box (6) is internally provided with a bearing substrate (9) for bearing and collecting nano-conductor or semiconductor materials.
2. The system for preparing nano-conductor or semiconductor material with controllable size according to claim 1, wherein: the tubular furnace (5) is any one of a single-temperature-zone tubular furnace, a double-temperature-zone tubular furnace and a multi-temperature-zone tubular furnace.
3. The system for preparing nano-conductor or semiconductor material with controllable size according to claim 1, wherein: the ablation reaction container (3) is provided with an air inlet pipeline (10) and a first air outlet pipeline (11), the ablation reaction container (3) is communicated to the inert gas source (4) through the air inlet pipeline (10), the ablation reaction container (3) is communicated to the tube furnace (5) through the first air outlet pipeline (11), the tube furnace (5) is provided with a second air outlet pipeline (12), the tube furnace (5) is communicated to the collecting device through the second air outlet pipeline (12), and the air inlet pipeline (10), the first air outlet pipeline (11) and the second air outlet pipeline (12) are all provided with one-way valves (13) for controlling the flow speed of the inert gas to be slow.
4. The system for preparing nano-conductor or semiconductor material with controllable size according to claim 3, wherein: the ablation reaction vessel (3) is a closed cuboid vessel, the two electrode fixing seats (8) are oppositely arranged at the upper wall and the lower wall of the ablation reaction vessel (3) from top to bottom, the air inlet pipeline (10) and the first air outlet pipeline (11) are oppositely arranged at the left wall and the right wall of the ablation reaction vessel (3) from left to right, the mounting axes of the two electrode fixing seats (8) are arranged on the same vertical straight line, the mounting axes of the air inlet pipeline (10), the first air outlet pipeline (11) and the second air outlet pipeline (12) are arranged on the same horizontal straight line, and the mounting axis of the electrode fixing seat (8) and the mounting axis of the air inlet pipeline (10) are intersected at the midpoint of the ablation reaction vessel (3).
5. The system for preparing nano-conductor or semiconductor material with controllable size according to claim 3, wherein: the collecting device further comprises a vertically arranged deposition pipeline (14), the upper end of the deposition pipeline (14) is communicated with the tail end of the second gas outlet pipeline (12), and the lower end of the deposition pipeline (14) is arranged right above the bearing substrate (9).
6. The system for preparing nano-conductor or semiconductor material with controllable size according to claim 4, wherein: the ablation reaction container (3) is provided with a first threaded hole (15) for installing the electrode fixing seat (8), the electrode fixing seat (8) comprises a fixing circular truncated cone (16), an adjusting screw rod (17) and an electrode base (18), the fixing circular truncated cone (16) is provided with an external thread (19) matched with the first threaded hole (15), the fixing circular truncated cone (16) is provided with a second threaded hole (20) matched with the adjusting screw rod (17) at the central shaft of the fixing circular truncated cone, and the electrode base (18) is fixedly connected to the tail end of the adjusting screw rod (17).
7. The system for preparing nano-conductor or semiconductor material with controllable size according to claim 6, wherein: the bottom end of the electrode base (18) is provided with a conducting strip (21) electrically connected with the power supply (1), and the side wall of the electrode base (18) is provided with a plurality of locking screw rods (22) used for clamping the electrodes (2).
8. The method for preparing nano conductor or semiconductor material with controllable size is characterized in that the nano conductor or semiconductor material with controllable size is prepared by the preparation system of any one of claims 1 to 7, and comprises the following preparation steps:
s1: the two electrodes (2) are respectively installed and fixed on the two electrode (2) fixing seats, the two electrodes (2) are adjusted to be in the same straight line, and the distance between the reaction end faces of the two electrodes (2) is 0.1-3 mm;
s2: opening an inert gas source (4), adjusting the flow rate of the inert gas, and smoothly introducing the inert gas into the ablation reaction container (3) for 3-5 mins;
s3: preheating the tube furnace (5) to enable the tube furnace (5) to reach a preset temperature;
s4: switching on a power supply (1), carrying out high-voltage spark ablation reaction on the electrodes (2) at two ends to produce nano conductor or semiconductor materials, and simultaneously, feeding the produced nano conductor or semiconductor materials into a tubular furnace (5) along with inert gas flow for heat treatment;
s5: the heat-treated nano conductor or semiconductor material enters the collection box (6) along with the inert gas flow and is deposited on the bearing substrate (9).
9. The method for preparing nano conductor or semiconductor material with controllable size according to claim 8, characterized in that: the temperature of the tubular furnace (5) is 20-1500 ℃, the inner diameter of the tubular furnace (5) is 1-500 mm, and the length of a heat treatment temperature zone of the tubular furnace (5) is 0.1-2 m.
10. The method for preparing nano conductor or semiconductor material with controllable size according to claim 8, characterized in that: the inert gas source (4) is any one of nitrogen, argon and helium, and the flow rate of the inert gas is 0.1-20L/min.
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| CN114029495B (en) * | 2021-11-17 | 2023-08-04 | 广东工业大学 | Preparation system and preparation method for preparing nano metal particles by low-temperature airflow |
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| WO2021136059A1 (en) | 2021-07-08 |
| CN111168076B (en) | 2020-10-27 |
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