A device and method for preparing high-energy-rate synthetic materials in gas phase

By setting copper wires and electrode plates in the reaction tube to form an electromagnetic field and using an igniter to perform detonation reaction, the preparation process of nanomaterials is simplified, and the problems of complex processes, long time and low yield in the existing technology are solved, and the problem of "complex" process, long time and low yield" is realized. Efficient, safe and large-scale nanomaterial production.

CN113457570BActive Publication Date: 2024-12-13GANSU NINGSHI IND
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Patent Information

Application Number
CN202110903551.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2021-08-06
Publication Date
2024-12-13
Estimated Expiration
2041-08-06

AI Technical Summary

Technical Problem

In the prior art, nanomaterial preparation processes are complex, have many procedures, take a long time and produce less, making it difficult to achieve large-scale production.

Method used

A gas-phase preparation device for high-energy synthetic materials is adopted. By setting copper wires and electrode plates in the reaction tube, an electromagnetic field is formed, and a detonation reaction is carried out using an igniter to generate nanomaterials, simplifying process steps and improving efficiency.

Benefits of technology

It realizes rapid, efficient and large-scale production of material preparation, ensuring the safety, reliability and cleanliness and environmental protection of the reaction.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention provides a gas phase preparation device and method for high energy efficiency synthetic materials, wherein a reaction tube is provided, an inner tube and a copper wire are provided in the reaction tube along the length direction thereof, an electrode plate is provided at each end of the reaction tube, and the reaction tube is also connected to a vacuum pump, a gas transmission pipe and a feeding pipe. The present invention performs a reaction in a detonation manner in the reaction tube and prepares nanomaterials, and the material preparation can be completed in one step, with fewer process steps, high efficiency and rapidity, and can be mass-produced nanomaterials; the detonation reaction is performed in a closed reaction tube, and the reaction process is safe, reliable, clean, environmentally friendly and pollution-free.
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Description

Technical Field

[0001] This invention belongs to the field of nanomaterial preparation technology, and relates to a high-energy-efficiency synthetic material gas-phase preparation apparatus and method. Background Technology

[0002] Conventional lithium-ion batteries use graphene as the anode material, but lithium-ion batteries have low capacity and can no longer meet the requirements of increasingly advanced application devices. Silicon, on the other hand, has a theoretical specific capacity of 3579 mAh / g and is a promising new generation of anode material.

[0003] However, silicon undergoes a 323% volume expansion during lithiation and delithiation, causing silicon particles to break and pulverize. This leads to the formation of a new SEI film between the electrolyte and the broken silicon, which in turn damages the electrode structure, interrupts electron and ion migration channels, and causes a rapid decline in electrode stability or even battery failure. Therefore, the commonly used technical approach is to nanoscale silicon materials to reduce the absolute value of volume expansion; furthermore, to make the silicon materials porous and foamed, allowing the expansion to extend inwards, reducing the external effects of expansion, creating ion migration channels, and increasing the surface area for adsorbed ions. Finally, graphene is used to coat silicon ions. Due to graphene's strong self-supporting ability and toughness, a bird's nest-like mesh structure can be constructed to create space to absorb silicon expansion. Currently, the above synthesis methods require multiple steps, are complex, involve many procedures, are time-consuming, and have low production volumes, making large-scale production difficult. Summary of the Invention

[0004] The purpose of this invention is to address the problems of complex, lengthy, and low-yield nanomaterial preparation processes in existing technologies, which make large-scale production difficult. The invention provides a safe, reliable, clean, environmentally friendly, fast, efficient, and scalable high-efficiency high-energy-rate gas-phase synthesis device and method for nanomaterials.

[0005] Therefore, the present invention adopts the following technical solution:

[0006] A high-energy-efficiency synthetic material gas-phase preparation apparatus, characterized in that it includes a reaction tube, each end of which is provided with a detachable sealing flange; a copper wire is arranged along the length of the reaction tube, the copper wire coinciding with the center line of the reaction tube; an electrode plate is provided at each end of the reaction tube, the electrode plate being located outside the sealing flange; an igniter is provided at one end of the reaction tube, the igniter being located on one of the sealing flanges; a gas supply main pipe is provided inside the reaction tube, the gas supply main pipe extending out of the reaction tube, the inner end of the gas supply main pipe forming a gas supply port; a vacuum tube and a gas supply branch pipe are connected to the outer end of the gas supply main pipe; a vacuum pump is connected to the vacuum tube; and a feeding pipe is also connected to the reaction tube, the feeding pipe being located at the upper part of the reaction tube.

[0007] Furthermore, an inner tube is provided inside the reaction tube along its length, the gas inlet extends into the inner tube from one end, and the igniter extends into the inner tube from the other end.

[0008] Furthermore, the gas supply branch pipe is connected to a gas mixing chamber, and a gas supply valve is provided on the gas supply branch pipe.

[0009] Furthermore, the reaction tube is equipped with a wave velocity measuring instrument and a piezoelectric sensor for measuring the velocity of the detonation shock wave.

[0010] Furthermore, the reaction tube is equipped with an electric heating tape and a temperature sensor.

[0011] Furthermore, a funnel is connected to the top of the feeding pipe, and a first valve is provided on the feeding pipe.

[0012] Furthermore, the reaction tube is connected to a medium gas input pipe, and a second valve is provided on the medium gas input pipe.

[0013] This invention also provides a method for the gas-phase preparation of high-energy-efficiency synthetic materials, comprising the following steps:

[0014] (1) Add a precursor and oxygen or hydrogen and oxygen to the reaction tube of any of the above high-energy-rate synthetic material gas phase preparation apparatus;

[0015] (2) When the copper wire is energized, a ring magnetic field is formed around the copper wire, and the electrode plate is activated, so that an electric field is formed inside the reaction tube.

[0016] (3) Start the igniter. The igniter has an energy of 30-60J. Ignite the gas in the reaction tube to detonate the precursor in the reaction tube and generate nanomaterials.

[0017] Further, in step (1), if the precursor is a gas, the reaction tube is first evacuated, and then the precursor and oxygen or hydrogen-oxygen mixture are added to the gas mixing chamber, mixed evenly, and then fed into the reaction tube.

[0018] If the precursor is solid, open the sealing flange at the end of the reaction tube, lay the precursor flat on the plate and place it into the reaction tube, install the flange, evacuate the reaction tube, and then add oxygen or hydrogen-oxygen mixture into the gas mixing chamber and input it into the reaction tube.

[0019] If the precursor is a liquid, add the precursor to the funnel, start the heating tape to heat the reaction tube and evacuate the reaction tube, then input the precursor from the funnel into the reaction tube, add oxygen or a hydrogen-oxygen mixture into the gas mixing chamber and then into the reaction tube.

[0020] Furthermore, the precursor is a mixture of acetylene, benzene, biphenyl, silicon, silicon dioxide and magnesium powder, or a mixture of acetylene and benzene.

[0021] The beneficial effects of this invention are as follows:

[0022] (1) The reaction is carried out in the reaction tube by detonation and nanomaterials are prepared. The material preparation can be completed in one step. The process steps are few, efficient and fast, and nanomaterials can be mass-produced.

[0023] (2) Before filling the reaction tube with gas, the reaction tube is evacuated to ensure the volume and proportion of the gas added and the pressure inside the reaction tube, thereby improving the preparation effect of nanomaterials.

[0024] (3) Install copper wires inside the reaction tube and install electrode plates on the connecting section of the reaction tube. Apply electric and magnetic fields to the reaction tube during the reaction to control the particle arrangement and improve the reaction effect.

[0025] (4) The detonation reaction is carried out in a closed reaction tube. The reaction process is safe, reliable, clean, environmentally friendly and pollution-free. Attached Figure Description

[0026] Figure 1 This is a schematic diagram of the structure of the high-energy-efficiency synthetic material gas-phase preparation apparatus of the present invention;

[0027] Figure 2 Scanning electron microscope image of graphene nanoparticles generated using acetylene as a precursor;

[0028] Figure 3 Scanning electron microscope image of graphene nanoparticles generated using biphenyl as a precursor;

[0029] Figure 4 This is a scanning electron microscope image of nanoporous silicon.

[0030] Figure 5 This is a scanning electron microscope image of nano-silicon;

[0031] Figure 6 Scanning electron microscope image of a mixture of silicon nanospheres and silicon nanowires;

[0032] Figure 7 Scanning electron microscope image of graphene-coated silicon particles;

[0033] In the diagram, 1-reaction tube, 2-sealing flange, 3-copper wire, 4-electrode plate, 5-igniter, 6-gas main pipe, 7-gas inlet, 8-vacuum tube, 9-gas branch pipe, 10-vacuum pump, 11-gas mixing chamber, 12-gas valve, 13-threading hole, 14-feeding pipe, 15-funnel, 16-first valve, 17-inner tube, 18-medium gas input pipe, 19-second valve, 20-heating tape, 21-temperature sensor, 22-wave velocity measuring instrument, 23-piezoelectric sensor, 24-inner tube support plate.

[0034] Specifically, in terms of implementation methods

[0035] The present invention will now be described in detail with reference to the accompanying drawings and embodiments:

[0036] Example 1

[0037] like Figure 1 As shown, a high-energy-rate synthetic material gas-phase preparation device includes a horizontally arranged reaction tube 1. The reaction tube 1 is made of thick-walled steel pipe with a volume of about 300L, an impact pressure resistance Pa / P0>45 (P0 is the initial working pressure), and a static pressure resistance of 10mPa. It is used to ensure that the detonation proceeds according to the rules and to collect the reaction products. Each end of the reaction tube 1 is provided with a detachable sealing flange 2. During use, either sealing flange 2 can be opened to add a solid precursor into the reaction tube 1. A copper wire 3 is arranged along the length of the reaction tube 1, and the copper wire 3 coincides with the center line of the reaction tube 1. Specifically, a wire hole 13 can be provided in the middle of the sealing flange 2 to pass the copper wire through the wire hole 13 in the middle of the sealing flange 2. Each end of the reaction tube 1 is provided with an electrode plate 4, which is located outside the sealing flange 2. The copper wire 3 and the electrode plate 4 can influence the magnetic field and electric field environment provided by the reaction. The magnetic field and electric field can affect the corresponding particle arrangement during the detonation reaction.

[0038] An igniter 5 is installed at one end of the reaction tube 1. The igniter 5 is a commonly used electronic igniter for detonation reactions. The igniter 5 is located on one of the sealing flanges 2. The ignition energy of the igniter 5 must be greater than 30J to ensure the occurrence of detonation. For safety, the power supply of the igniter 5 must be disconnected and the ignition point grounded during operation. A gas supply pipe 6 is installed inside the reaction tube 1. The gas supply pipe 6 extends out of the reaction tube 1. Specifically, in this embodiment, it extends out of the sealing flange 2 at the end away from the igniter 5. The inner end of the gas supply pipe 6 is located inside the reaction tube 1 and forms a gas supply port. 7. The outer end of the main gas supply pipe 6 is connected to a vacuum pipe 8 and a gas supply branch pipe 9. The vacuum pipe 8 is connected to a vacuum pump 10. The vacuum pump 10 can evacuate the reaction tube 1 through the vacuum pipe 8 and the main gas supply pipe 6. The purpose of evacuating the vacuum is to ensure the accuracy of the raw material ratio and to eliminate impurities. The gas supply branch pipe 9 is used to supply reaction gas into the reaction tube 1. The gas supply branch pipe 9 is connected to a gas mixing chamber 11. When supplying gas to the reaction tube 1, the gas can be mixed evenly through the gas mixing chamber 11 before being supplied. In addition, the gas supply branch pipe 9 is equipped with a gas supply valve 12, which is used to prevent...

[0039] For ease of use, the reaction tube 1 is also connected to a feed tube 14, which is located at the top of the reaction tube 1. The feed tube 14 is used to add liquid raw materials into the reaction tube 1. A funnel 15 is connected to the top of the feed tube 14, and a first valve 16 is also provided on the feed tube 15.

[0040] The reaction tube 1 is detachably equipped with an inner tube 17 along its length. Specifically, the reaction tube 1 has two inner tube support plates 24. The top of the inner tube support plate 24 has an arc-shaped structure adapted to the inner tube 17. The inner tube support plate 24 is used to support the inner tube 17 and is located at both ends of the inner tube 17. The inner tube 17 is made of a fragile material. The inner tube 17 allows the product to disperse radially and react with the detonation medium in a secondary reaction. At the same time as dispersion, it can also accelerate the cooling of the product. The gas inlet 7 extends into the inner tube 17 from one end of the inner tube 17, and the igniter 5 extends into the inner tube 17 from the other end of the inner tube 17.

[0041] The reaction tube 1 is connected to a medium gas input pipe 18, and a second valve 19 is provided on the medium gas input pipe 18.

[0042] In addition, the reaction tube 1 is equipped with an electric heating tape 20 and a temperature sensor 21. The electric heating tape 20 can heat the inside of the reaction tube 1, thereby increasing the initial temperature of the reaction and causing the liquid raw materials to vaporize. The temperature sensor 21 is used to measure the temperature inside the reaction tube 1. The temperature should be controlled below 300 degrees during heating.

[0043] The reaction tube 1 is equipped with a wave velocity measuring instrument 22 for measuring the detonation shock wave velocity, and a piezoelectric sensor 23.

[0044] This invention also provides a method for the gas-phase preparation of high-energy-efficiency synthetic materials. The method is described in detail below with reference to the embodiments:

[0045] This method prepares nano-graphene by selecting acetylene or biphenyl with hexacyclic carbon groups as precursors. When the hexacyclic carbon is subjected to impact compression, it will bend and fold, and the C-C bonds will be compressed or elongated. It will respond to pressure and temperature, thereby producing nano-graphene sheets, carbon nanotubes or fullerenes. The graphene formation window is T=3200-3800k and P=13-18atm.

[0046] Example 2

[0047] (1) Using gaseous acetylene as a precursor, acetylene and oxygen are added to the gas mixing chamber 11, and the mixed gas in the gas mixing chamber 11 is balanced with negative oxygen. The vacuum pump 10 is started to evacuate the reaction tube 1. The purpose of evacuation is to ensure the accuracy of the raw material ratio and to eliminate impurities in the reaction tube 1. After evacuation, the mixed gas in the gas mixing chamber 11 is input into the reaction tube 1, so that P0=0.1MPa in the reaction tube 1.

[0048] (2) When the copper wire 3 is energized, a ring magnetic field is formed around the copper wire 3, and the electrode plate 4 is activated to form an electric field inside the reaction tube 1.

[0049] (3) Start the igniter 5. The energy of the igniter 5 is 40. The mixed gas in the reaction tube 1 is ignited to detonate the precursor acetylene in the reaction tube 1 to generate nano-graphene. After the product cools down, open the sealing flange 2 with the igniter 5 to take out the product.

[0050] Scanning electron microscopy (SEM) images of acetylene-based graphene nanoparticles were obtained by microelectron scanning (see [link]). Figure 2 Observation shows that the graphene prepared by acetylene is a bowl-shaped spherical particle with deep curvature and increased thickness of each sheet. At the same time, since the precursor used was not subjected to acid heat treatment, the graphene surface has no functional groups and is in a primitive state.

[0051] Example 3

[0052] (1) Using solid biphenyl as a precursor, take 100g of flaky crystalline biphenyl with a particle size of less than 10μm and lay it on a plate with an average thickness of 2mm. Then open the sealing flange 2 and place it into the reaction tube 1. Close the sealing flange 2 and start the vacuum pump 8 to evacuate the reaction tube 1. Use oxygen filling to evacuate the vacuum so that the residual air in the reaction tube 1 is less than 2%. After evacuation, inject hydrogen and oxygen into the mixing chamber 11 in a ratio of 2:1 and mix them. Then inject the mixed gas into the reaction tube 1 so that P0=0.2MPa in the reaction tube 1.

[0053] (2) When the copper wire is energized, a ring magnetic field is formed around the copper wire, and the electrode plate is activated to form an electric field inside the reaction tube.

[0054] (3) Ignite 5 is started. The energy of igniter 5 is 40. The hydrogen-oxygen mixture in reaction tube 1 is ignited to detonate the biphenyl precursor in reaction tube 1. The detonation wave slightly sweeps the biphenyl layer, causing it to dehydrogenate thermally and generate nano-graphene. After the product cools down, the sealing flange 2 is opened and the product is taken out. During this process, the relevant sensors measured the detonation wave temperature to be 3583k, the pressure P / Po=17.5, and the velocity to be 2800m / s.

[0055] Scanning electron microscopy (SEM) images of graphene nanoparticles generated using biphenyl as a precursor were obtained by microelectron scanning (see...). Figure 3 Observation shows that the graphene generated by biphenyl as a precursor has large sheets and a large surface curvature with little wrinkling.

[0056] Example 4

[0057] (1) Using liquid benzene as a precursor, 100 mL of benzene is injected into funnel 15. Then, the heating tape 20 is started to preheat the reaction tube 1. The temperature in the reaction tube 1 is controlled to 85 degrees by temperature sensor 21. Then, the vacuum pump 8 is started to evacuate the reaction tube 1. The reaction tube 1 is evacuated to P=-0.084 MPa. Then, the first valve 16 is opened so that the liquid benzene in funnel 15 is slowly dripped into the reaction tube 1 through feeding pipe 14 (at this time, the reaction tube 1 is under negative pressure. Benzene enters the reaction tube 1 through feeding pipe 14 under the action of external air pressure). After all the benzene has entered the reaction tube 1, the first valve 16 is immediately closed. Since the temperature in the reaction tube 1 is 85 degrees, the benzene is completely vaporized after entering the reaction tube 1. Then, oxygen is introduced into the mixing chamber 11 and the oxygen is introduced into the reaction tube 1 through the gas supply branch pipe 9 and the gas supply main pipe 6 so that P0=0.08 MPa in the reaction tube 1.

[0058] (2) When the copper wire 3 is energized, a ring magnetic field is formed around the copper wire 3, and the electrode plate 4 is activated to form an electric field inside the reaction tube 1.

[0059] (3) Start igniter 5. The energy of igniter 5 is 40. Ignite the gaseous benzene and oxygen mixture in reaction tube 1 to detonate the gaseous benzene precursor in reaction tube 1 to generate nano-graphene. After the product cools down, open the sealing flange 2 to take it out.

[0060] The purpose of preparing nanoporous silicon using this method is that although silicon has a high capacity of 3600 mAh / g, when used as a negative electrode in lithium-ion batteries, it will produce a volume expansion of 323% during the lithiation or delithiation process, which will destroy the electrode structure. Therefore, it is necessary to overcome the volume effect of silicon and increase the electron transport channels within the silicon particles.

[0061] Example 5

[0062] Using silica and magnesium powder as precursors, 15g of silica and 11g of magnesium powder are mixed and stirred evenly, and a thin layer is spread on a plate. Then, the sealing flange 2 is opened and the mixture is placed into the reaction tube 1. The sealing flange 2 is closed, and the vacuum pump 10 is started to evacuate the reaction tube 1 through the vacuum tube 8 and the gas supply pipe 6, so that P=-0.080mpa. After the evacuation is completed, hydrogen and oxygen are injected into the mixing chamber 11 in a 2:1 ratio and mixed. Then, the mixed gas is injected into the reaction tube 1, so that P0=0.5mpa in the reaction tube 1.

[0063] (2) When the copper wire 3 is energized, a ring magnetic field is formed around the copper wire 3, and the electrode plate 4 is activated to form an electric field inside the reaction tube 1.

[0064] (3) Start the igniter 5. The energy of the igniter 5 is 40. Ignite the gas in the reaction tube 1 to detonate the precursor in the reaction tube 1 and generate nanoporous silicon. Some magnesium oxide will be mixed in the porous silicon. After the product cools down, open the sealing flange 2 and take it out.

[0065] The principle of pore formation in silicon in this embodiment is as follows: SiO2 + 2Mg = Si + 2MgO. When the mixed gas 2H2 + O2 is detonated, the temperature reaches 3583K, causing SiO2 to boil (the boiling point of SiO2 is 3220K) and undergo a redox reaction with Mg (the boiling point of Mg is 368K) to produce MgO (the melting point of MgO is 3099K and the boiling point is 3873K). This allows MgO to be trapped in Si to form pores. After the product solidifies, the MgO trapped in Si is dissolved with hydrochloric acid, and finally nanoporous silicon is obtained.

[0066] The obtained nanoporous silicon was subjected to microelectronic scanning to obtain scanning electron microscopy images (see...). Figure 4 As can be seen, the pores inside the silicon are dense and uniform.

[0067] Preparation of silicon nanoparticles and nanowires.

[0068] Example 6

[0069] (1) Using silicon particles as precursors, take 5μm pure silicon particles, spread them in a thin layer on a plate, then open the sealing flange 2 and place them into the reaction tube 1, close the sealing flange 2, start the vacuum pump 10 to evacuate the reaction tube 1 through the vacuum tube 8 and the gas supply pipe 6, after the evacuation is completed, inject hydrogen and oxygen into the mixing chamber 10 in a ratio of 2:1 and then inject the mixed gas into the reaction tube 1 so that P0=0.5mpa in the reaction tube 1;

[0070] (2) When the copper wire 3 is energized, a ring magnetic field is formed around the copper wire 3, and the electrode plate 4 is activated to form an electric field in the reaction tube 1.

[0071] (3) Start the igniter 5. The igniter has an energy of 40. Ignite the hydrogen-oxygen mixture in the reaction tube 1 to detonate the pure silicon particle precursor in the reaction tube 1, generating spherical nano-silicon particles. After the product cools down, finally open the sealing flange 2 to take it out.

[0072] The obtained nano-silicon was subjected to microelectronic scanning to obtain scanning electron microscopy images (see...). Figure 5 As can be seen, silicon is spherical.

[0073] Example 7

[0074] (1) Using silicon particles as precursors, the inner tube 17 is installed in the reaction tube 1. Take 5μm pure silicon particles, spread them in a thin layer on a plate, and then open the sealing flange 2 to place them into the inner tube 17. Close the sealing flange 2 and start the vacuum pump 10 to evacuate the inner tube 17 and the reaction tube 1. After evacuation, argon gas is introduced into the reaction tube 1 through the medium gas input pipe 18 as the medium gas and the P0 in the reaction tube 1 is made to be 0.8 mpa. Hydrogen and oxygen are injected into the mixing chamber 11 in a 2:1 ratio to mix. Then the mixed gas is injected into the inner tube 17 so that the P0 in the inner tube 17 is 0.5 mpa.

[0075] (2) When the copper wire 3 is energized, a ring magnetic field is formed around the copper wire 3, and the electrode plate 4 is activated to form an electric field inside the reaction tube 1.

[0076] (3) Start the igniter 5. The energy of the igniter 5 is 40. The gas in the reaction tube 1 is ignited to detonate the silicon particle precursor in the inner tube 17. The detonation causes the inner tube 17 to break. The reaction products are scattered radially along the inner tube 17 in the reaction tube 1. Under the argon anti-oxidation environment, a mixture of nanospheres and nanowires is obtained. After the product cools down, the sealing flange 2 is opened and the product is taken out.

[0077] The obtained mixture of silicon nanospheres and silicon nanowires was subjected to microelectronic scanning to obtain scanning electron microscopy images (see...). Figure 6 As can be seen, silicon exists in spherical and filamentous forms.

[0078] This method was used to prepare graphene-coated silicon nanoparticles.

[0079] Example 8

[0080] Using silicon particles and acetylene as precursors, 80g of pure silicon was spread in a thin layer on a flat plate. Then, the sealing flange 2 was opened and the silicon was placed into the reaction tube 1. The sealing flange 2 was closed and the vacuum pump 10 was started to evacuate the reaction tube 1. After evacuation, acetylene and oxygen were injected into the mixing chamber 11 at a ratio of 3:1 and mixed. Then, the mixed gas was injected into the reaction tube 1, so that P0=0.1MPa in the reaction tube 1.

[0081] (2) When the copper wire 3 is energized, a ring magnetic field is formed around the copper wire 3, and the electrode plate 4 is activated to form an electric field inside the reaction tube 1.

[0082] (3) Start the igniter 5. The igniter has an energy of 40. Ignite the acetylene and oxygen mixture in the reaction tube 1 to detonate the acetylene and pure silicon precursor in the reaction tube 1 to generate graphene-coated nano-silicon. After the product cools down, finally open the sealing flange 2 to take it out.

[0083] The principle of this reaction is that 3C2H2 + O2 slightly sweeps the silicon layer (silicon's bp 3538k, mp 1687k) under P0 = 0.1 MPa. The silicon is vaporized into droplets that float in reaction tube 1. At the same time, acetylene reacts to form graphene, which fills the entire reaction tube 1. At this time, the silicon droplets are surrounded by the graphene environment. After condensation, they form graphene-coated silicon particles, thus completing the aerosol gelation process.

[0084] The obtained graphene-coated silicon product was subjected to microelectronic scanning to obtain scanning electron microscopy (SEM) images (see...). Figure 7 As can be seen, the silicon particles are spherical (black), and graphene (white) is uniformly coated on the outer surface of the silicon spheres.

Claims

1. A gas phase preparation device for high energy efficiency synthetic materials, It is characterized in that The invention comprises a reaction tube, wherein a detachable sealing flange is respectively arranged at both ends of the reaction tube, a copper wire is arranged inside the reaction tube along the length direction thereof, the copper wire coincides with the center line of the reaction tube, an electrode plate is respectively arranged at both ends of the reaction tube, the electrode plate is located outside the sealing flange, an igniter is arranged at one end of the reaction tube, the igniter is located on one of the sealing flanges, a gas main pipe is arranged inside the reaction tube, the gas main pipe passes through the reaction tube, a gas delivery port is formed at the inner end of the gas main pipe, a vacuum pipe and a gas delivery branch pipe are connected to the outer end of the gas main pipe, the vacuum pipe is connected to a vacuum pump, the reaction tube is also connected to a feeding pipe, the feeding pipe is located at the upper part of the reaction tube, an inner pipe is arranged inside the reaction tube along the length direction thereof, the gas delivery port extends into the inner pipe from one end of the inner pipe, and the igniter extends into the inner pipe from the other end of the inner pipe.

2. A gas phase preparation device for high energy efficiency synthetic materials according to claim 1, It is characterized in that The gas transmission branch pipe is connected to a gas mixing chamber, and a gas transmission valve is arranged on the gas transmission branch pipe.

3. A high-efficiency synthetic material gas phase preparation device according to claim 1, It is characterized in that The reaction tube is provided with a wave velocity measuring instrument and a piezoelectric sensor for measuring the velocity of the detonation shock wave.

4. A gas phase preparation device for high energy efficiency synthetic materials according to claim 1, It is characterized in that The reaction tube is provided with an electric heating belt and a temperature sensor.

5. A gas phase preparation device for high energy efficiency synthetic materials according to claim 1, It is characterized in that The top of the feeding pipe is connected with a funnel, and the feeding pipe is provided with a first valve.

6. A gas phase preparation device for high energy efficiency synthetic materials according to claim 1, It is characterized in that The reaction tube is connected with a medium gas input pipe, and a second valve is arranged on the medium gas input pipe.

7. A gas phase preparation method for high energy efficiency synthetic materials, It is characterized in that The following steps are involved: (1) Adding a precursor and oxygen or a mixture of hydrogen and oxygen into a reaction tube of a gas phase preparation device for high energy efficiency synthetic materials according to any one of claims 1 to 6; (2) Power is applied to the copper wire to form a circular magnetic field around the copper wire, and the electrode plate is activated to form an electric field in the reaction tube; (3) Start the igniter, the energy of which is 30-60 J, to ignite the gas in the reaction tube, causing the precursor in the reaction tube to detonate and generate nanomaterials.

8. A gas phase preparation method for high energy efficiency synthetic materials according to claim 7, It is characterized in that In the step (1), if the precursor is a gas, the reaction tube is first evacuated, and then the precursor and oxygen or hydrogen-oxygen mixed gas are added into the gas mixing chamber, mixed evenly, and then input into the reaction tube; If the precursor is solid, open the sealing flange at the end of the reaction tube, spread the precursor on a flat plate and place it in the reaction tube, install the flange, evacuate the reaction tube, and then add oxygen or hydrogen-oxygen mixed gas into the gas mixing chamber and input it into the reaction tube; If the precursor is liquid, add the precursor into the funnel, start the electric heating belt to heat the reaction tube and evacuate the reaction tube, then input the precursor in the funnel into the reaction tube, add oxygen or hydrogen and oxygen mixed gas into the gas mixing chamber, and input it into the reaction tube.