WO2020034090A1 - 纳米材料制备设备和方法 - Google Patents

纳米材料制备设备和方法 Download PDF

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Publication number
WO2020034090A1
WO2020034090A1 PCT/CN2018/100442 CN2018100442W WO2020034090A1 WO 2020034090 A1 WO2020034090 A1 WO 2020034090A1 CN 2018100442 W CN2018100442 W CN 2018100442W WO 2020034090 A1 WO2020034090 A1 WO 2020034090A1
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Prior art keywords
reaction furnace
crucible
furnace
cooling
gas
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PCT/CN2018/100442
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English (en)
French (fr)
Inventor
胡军辉
葛大梁
Original Assignee
深圳市百柔新材料技术有限公司
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Application filed by 深圳市百柔新材料技术有限公司 filed Critical 深圳市百柔新材料技术有限公司
Priority to PCT/CN2018/100442 priority Critical patent/WO2020034090A1/zh
Publication of WO2020034090A1 publication Critical patent/WO2020034090A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/12—Making metallic powder or suspensions thereof using physical processes starting from gaseous material

Definitions

  • the invention belongs to the technical field of nano material preparation, and particularly relates to a nano material preparation device and method.
  • Nanomaterials Materials that control the size of the constituent phase or grain structure below 100nm are called nanomaterials, that is, at least one dimension in three-dimensional space is in the unit of nanoscale (1 ⁇ 100nm) or is constructed by them according to a certain rule.
  • Materials or structures are defined as nanomaterials.
  • Nanomaterials have volume effects, surface effects, quantum size effects, quantum tunneling effects, and dielectric confinement effects. These effects have resulted in many physical and chemical properties of nanomaterials such as melting point, vapor pressure, optical properties, magnetic properties, superconductivity, and plastic deformation. Aspects have shown special performance. These special properties make nanomaterials a new research hotspot in many fields such as electricity, magnetism, mechanics, catalysis and biomedicine.
  • the preparation of nanomaterials mostly uses chemical methods and physical methods.
  • Chemical methods include chemical vapor phase reaction, chemical vapor deposition, precipitation method, hydrothermal method, sol-gel method, and chemical reduction method.
  • the disadvantages of the chemical method are that a solvent is used in the preparation process, the preparation is prone to produce impurities, and the finally formed nano powder is easy to aggregate, difficult to separate, and has poor sphericity, and the process for preparing the nano alloy material is complicated.
  • Physical preparation methods include mechanical pulverization, vapor phase evaporation, and sputtering.
  • the disadvantage of mechanically pulverizing nano-particles is that the grain size is not uniform and it is easy to introduce certain impurities.
  • the vapor phase evaporation method currently has resistance heating, high frequency induction heating, arc discharge heating, laser heating, and plasma heating.
  • Vapor phase evaporation mainly uses a heating method, such as resistance heating and high-frequency induction heating. This method is more difficult to prepare high melting point and low vapor pressure substances.
  • the disadvantage of using arc discharge heating is that it is easy to generate electrode particles of micron size. Splashing, laser heating and plasma heating can be used to prepare metal, alloy or metal compound nanoparticles, but simply using a form of heat source, the energy consumption is high, and for the metal or alloy nano preparation process with low melting point and high vapor pressure The process is not well controlled.
  • For the physical evaporation method most of the high temperature resistant crucibles are used.
  • nanomaterials In the process of preparing nanomaterials, most nanomaterials need to be above 2000 ° C to evaporate quickly. Such high temperatures will cause some materials to react with the crucible. At the same time, the nano-powder prepared by physical method is in a dry state. Because the metal nano-powder is very active, in order to prevent it from spontaneously igniting due to rapid oxidation in direct exposure to air, it is common practice to pass appropriate oxygen to the alloy material before collection The surface is passivated, but this process takes a long time, and the surface passivation is difficult to judge and control.
  • the objective of the embodiments of the present application is to provide a nanomaterial preparation device, which aims to solve the technical problems that are easy to cause pollution during the preparation of high-purity nanomaterials and that the proportion of components is likely to be lost during the preparation of alloy nanomaterials.
  • a method for preparing nanomaterials which aims to solve the technical problems that are easy to bring pollution during the preparation of high-purity nanomaterials and that the proportion of components is likely to be lost during the preparation of alloy nanomaterials.
  • a nano material preparation equipment including:
  • An evacuation device connected to the reaction furnace and configured to evacuate the reaction furnace
  • a protective gas input device which is connected to the reaction furnace and is used to pass in a protective gas into the reaction furnace;
  • a magnetic levitation heating device which is arranged in the reaction furnace and is located on the outer periphery of the crucible and performs magnetic levitation heating on the raw materials in the crucible;
  • a laser heating device which is disposed outside the reaction furnace and its laser emitting end is directly opposite the reaction furnace and is configured to emit laser light to heat the raw material in the crucible so that the raw material evaporates to form atom / molecular vapor;
  • a cooling gas input device is connected to the reaction furnace, and the gas output end of the cooling gas input device is directly opposite the opening of the crucible and is used for passing in cooling gas to align the atomic / molecular vapor suspended in the crucible. Cooling to form nanomaterials;
  • a liquid-phase capture device is connected to the reaction furnace and is used to extract the nano-material into a liquid for further cooling.
  • a nano material preparation equipment including:
  • An evacuation device connected to the reaction furnace and configured to evacuate the reaction furnace
  • a protective gas input device which is connected to the reaction furnace and is used to pass in a protective gas into the reaction furnace;
  • a magnetic levitation heating device which is arranged in the reaction furnace and is located on the outer periphery of the crucible and performs magnetic levitation heating on the raw materials in the crucible until the raw materials are evaporated to form atom / molecular vapor;
  • a cooling gas input device is connected to the reaction furnace, and the gas output end of the cooling gas input device is directly opposite the opening of the crucible and is used for passing in cooling gas to align the atomic / molecular vapor suspended in the crucible. Cooling to form nanomaterials;
  • a liquid-phase capture device is connected to the reaction furnace and is used to extract the nano-material into a liquid for further cooling.
  • a method for preparing a nano material including the following steps:
  • a method for preparing a nano material including the following steps:
  • the present application has the following beneficial effects:
  • the nanomaterial preparation device of the present invention in the specific operation, firstly, raw materials are added to the crucible in the reaction furnace, and then the reaction furnace is evacuated by a vacuum extraction device, and then passed through The protective gas input device passes the protective gas into the reaction furnace in a vacuum state. Then, the crucible is magnetically suspended and heated by a magnetic suspension heating device until the raw material is melted and suspended in the crucible, and then the raw material suspended in the crucible is processed by a laser heating device.
  • the laser is heated until the raw material evaporates the atom / molecular vapor, the cooling gas input device passes in the cooling gas to rapidly cool the atom / molecular vapor suspended in the crucible to form a nanomaterial, and finally the liquid phase capture device extracts the nanomaterial to The liquid is further cooled and the nanomaterial is collected.
  • the raw materials are suspended in the crucible and separated from the crucible during the magnetic levitation heating process, thereby ensuring that there is no pollution source during the entire preparation process and ensuring the production of high-purity nanomaterials; In a short time, the local heating of the substance to an extremely high temperature and the evaporation of the substance will occur.
  • the substance that is evaporated can still maintain its original element ratio; and the evaporated nanomaterial is cooled by extraction into the liquid
  • the process of passivation of nano-materials is omitted, the production link is reduced, and the production cycle is shortened.
  • the raw materials are suspended in the crucible during heating and evaporation and separated from the crucible, thereby ensuring that the nanomaterial evaporated during the preparation process can still maintain its original element ratio.
  • FIG. 1 is a schematic structural diagram of a nanomaterial preparation device according to an embodiment of the present invention.
  • FIG. 2 is a flowchart of a method for preparing a nanomaterial provided in Embodiment 3 of the present invention.
  • FIG. 3 is a flowchart of a method for preparing a nanomaterial according to a fourth embodiment of the present invention.
  • thermometer 73 vacuum generator 74
  • thermometer 80 cooling gas input device
  • first and second are used for descriptive purposes only, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined as “first” and “second” may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "plurality” is two or more, unless specifically defined otherwise.
  • the terms “installation”, “connected”, “connected”, “fixed” and other terms shall be understood in a broad sense unless otherwise specified and defined, for example, they may be fixed connections or removable connections , Or integrated; it can be mechanical or electrical connection; it can be directly connected, or it can be indirectly connected through an intermediate medium, it can be the internal connection of the two elements or the interaction between the two elements.
  • the specific meanings of the above terms in the present invention can be understood according to specific situations.
  • Embodiment 1 Embodiment 1 .
  • a nanomaterial preparation device provided in this embodiment includes:
  • the reaction furnace 10 is a closed structure that can provide a working environment and installation support for the entire equipment.
  • the reaction furnace 10 can be operated at a high temperature, and has the advantages of high temperature resistance and high sealability.
  • the crucible 20 is set in the reaction furnace 10 and is used for containing raw materials.
  • the raw materials are generally metal powders. It is made of high temperature resistant materials.
  • the evacuation device 30 is connected to the reaction furnace 10 and is used to evacuate the inside of the reaction furnace 10.
  • the connection between the vacuum pumping device 30 and the reaction furnace 10 is sealed to avoid affecting the normal use of the vacuum pumping device 30 or the vacuum pumping effect in the reaction furnace 10 due to air tightness at the interface.
  • the vacuum evacuating device 30 is a device capable of evacuating the inside of the reaction furnace 10. During the specific work process, the original vacuum inside the reaction furnace 10 is sucked away by generating a negative pressure.
  • the protective gas input device 40 is connected to the reaction furnace 10 and is used to pass the protective gas into the reaction furnace 10; the connection between the protective gas input device 40 and the reaction furnace 10 is sealed to ensure that the protective gas is passed to the reaction. Air leakage occurred in the furnace 10.
  • the shielding gas may be argon, nitrogen, or the like. Among them, the protective gas such as argon and nitrogen is used to protect the raw materials in the crucible 20 from other qualitative changes such as oxidation, and to ensure normal heating and evaporation of the raw materials.
  • a magnetic levitation heating device 50 is provided in the reaction furnace 10 and is located on the outer periphery of the crucible 20 and performs magnetic levitation heating on the raw materials in the crucible 20.
  • the magnetic levitation heating device 50 can realize magnetic levitation induction heating.
  • the raw materials in the crucible 20 are suspended in the crucible 20; on the other hand, the raw materials can be heated so that the raw materials are heated to a temperature close to the boiling point.
  • the laser heating device 60 is disposed outside the reaction furnace 10 and the laser emitting end of the laser heating device 60 is directly opposite the reaction furnace 10 and is used to emit laser light to heat the raw materials in the crucible 20 so that the raw materials are evaporated to form Atom / Molecular Vapor.
  • the laser heating device 60 heats the raw material suspended in the crucible 20. At this time, the temperature of the raw material is close to the boiling point under the heating of the magnetic levitation heating device 50. Then, the laser heating device 60 further heats the laser quickly, and the laser heating device 60 generates The energy density of the laser feedstock quickly rises above the boiling point.
  • the cooling gas input device 80 is connected to the reaction furnace 10, and the gas output end of the cooling gas input device 80 is directly opposite to the opening of the crucible 20 and is used to pass cooling gas to the suspension of the crucible 20.
  • the atomic / molecular vapor is cooled to form a nanomaterial.
  • the gas output end of the cooling gas input device 80 is generally a tubular structure, and it only needs to extend above the crucible 20.
  • the cooling gas is first passed through the cooling gas input device 80 to the furnace body 11 to rapidly cool the evaporated substances. Nanomaterials that form the substance.
  • the cooling gas to be passed in may be a cooling gas such as nitrogen or carbon dioxide.
  • the liquid-phase capture device 70 is connected to the reaction furnace 10 and is used to extract the nano-material into a liquid for further cooling.
  • the evaporated nano-material is quickly extracted into the liquid through the liquid-phase trapping device 70 to be cooled, so as to avoid further growth of the nano-material, meanwhile, the process of passivation is omitted, and the collection is finally achieved.
  • the raw materials are first added to the crucible 20 in the reaction furnace 10, and then the reaction furnace 10 is evacuated by the vacuum extraction device 30, and then protected by The gas input device 40 passes protective gas into the reaction furnace 10 in a vacuum state, and then magnetically suspends and heats the crucible 20 through a magnetic levitation heating device 50 until the raw material melts and suspends in the crucible 20, and then suspends the The raw material in the crucible 20 is heated by laser until the raw material is evaporated to form atom / molecular vapor.
  • the cooling gas input device 80 is passed into the cooling gas to rapidly cool the atom / molecular vapor suspended in the crucible 20 to form a nano material.
  • the phase trapping device 70 further cools by extracting the nanomaterial into a liquid, and collects the nanomaterial.
  • the raw materials are suspended in the crucible 20 and separated from the crucible 20 during the magnetic levitation heating process, thereby ensuring that there is no pollution source during the entire preparation process and ensuring the production of high-purity nanomaterials; and because the high-energy laser beam can In a short period of time, the substance is locally heated to an extremely high temperature and the substance is evaporated. In the process, the substance that is evaporated can still maintain its original element ratio.
  • the evaporated nanomaterial is cooled by being extracted into a liquid to prevent the nanomaterial from growing further. At the same time, the process of passivating the nanomaterial is omitted, the production process is reduced, and the production cycle is shortened.
  • the crucible 20 is preferably a water-cooled copper crucible 20.
  • it can withstand high temperatures, on the other hand, it can avoid chemical reactions with raw materials. This can ensure that the evaporated nanomaterials have high purity and can maintain the original element ratio.
  • the crucible 20 can also be manufactured by using other materials that do not chemically react with the raw materials and have high-temperature performance, which will not be detailed here.
  • the magnetic levitation heating device 50 includes a coil capable of making the raw materials in the crucible 20 in a suspended state.
  • the coil can be wound on the outer wall of the crucible 20, and the coil can also realize the function of heating the raw materials.
  • the magnetic levitation heating device 50 may further include a resistor or other heating element that specifically heats the raw materials in the crucible 20, which may assist in heating the raw materials suspended in the crucible 20.
  • the reaction furnace 10 includes a furnace body 11, a furnace cover 12, and a furnace door 13, and a top opening (not shown in the figure) and a side opening (not shown in the figure) are provided on the top and the side of the furnace body 11, respectively.
  • the side opening is preferably opened on the front side of the nano material preparation equipment in a placed state, so as to facilitate the operation of the staff.
  • the furnace cover 12 is connected to the top of the furnace body 11 and is closed on the top opening.
  • the furnace cover 12 is movably connected to one edge of the top opening, so that it is convenient to open the furnace cover 12 and close the furnace cover 12 Can completely seal the top opening.
  • the furnace door 13 is connected to the side of the furnace body 11 and is closed on the side opening.
  • the furnace door 13 is movably connected to one side edge of the side opening, which facilitates opening the furnace door 13 and closing the furnace.
  • the door 13 can be completely closed behind the side opening.
  • opening the furnace cover 12 can facilitate the installation of various devices located in the furnace body 11 and the inspection and maintenance of each device. Opening the furnace door 13 can facilitate the addition of raw materials to the crucible 20.
  • the protective gas input device 40, the magnetic levitation heating device 50, and the liquid phase capture device 70 are connected to the side of the furnace body 11, and the laser heating device 60 is disposed above the furnace cover 12.
  • a laser inlet 113 is provided on the furnace cover 12 of the reaction furnace 10, and a laser emitting end of the laser heating device 60 is directly opposite to the laser inlet 113.
  • the laser inlet 113 is provided for the laser light emitted by the laser heating device 60 disposed above the furnace cover 12 to pass through. The laser light passing through the laser inlet 113 can further heat the raw materials suspended in the crucible 20 until the The temperature of the raw material reaches above the boiling point and evaporates.
  • an air blowing device 130 is provided in the reaction furnace 10 at a side of the laser inlet 113 to blow air toward the laser inlet 113 to prevent powder from accumulating in the laser inlet 113.
  • the setting of the blowing device 130 can blow gas to the laser inlet 113, so that the powder drama in the furnace body 11 can prevent the laser from passing through the laser inlet 113, and improve the stability and reliability of the laser heating device 60.
  • the blowing device 130 may be a fan.
  • observation window 131 is provided on the furnace door 13.
  • the observation window 131 is a transparent window, and its function is for the staff to observe and monitor the state in the furnace body 11 through the observation window 131 during the whole preparation process, so as to judge the change state of the raw materials in the process of preparing the nano powder.
  • the furnace body 11 has a double-layer stainless steel structure, and the inner layer has a cooling structure.
  • the furnace cover 12 has a double-layer stainless steel structure, and the inner layer has a cooling structure.
  • the furnace door 13 has a double-layer stainless steel structure, and the inner layer has a cooling structure.
  • cooling gas input device 80 is connected to the side of the furnace body 11 of the reaction furnace 10, and the interface is sealed to avoid leakage of air when the cooling gas is passed into the reaction furnace 10.
  • the nano-material preparation device further includes an infrared temperature measuring device 90.
  • the infrared temperature measuring device 90 is disposed outside the reaction furnace 10, and the reaction furnace 10 is provided with the infrared temperature measurement device.
  • the infrared rays projected by the device 90 pass through a glass window 111 to detect the temperature of the material in the crucible 20.
  • the glass window 111 is preferably disposed on the furnace cover 12.
  • the infrared temperature measuring device 90 can emit infrared rays to be projected into the crucible 20 through the glass window 111 provided on the furnace cover 12 to monitor the temperature of the raw materials in the crucible 20 in real time and sense the magnetic levitation heating device 50 according to the material evaporation temperature.
  • the temperature of the material in the crucible 20 is controlled within a reasonable range during heating to prevent some low boiling point and high vapor pressure components in the raw material from evaporating in advance, which causes the composition ratio of the alloy powder to be out of balance. It is mainly used in conjunction with the magnetic suspension heating device 50.
  • the infrared temperature measuring device 90 may be connected to the furnace cover 12 through a fixed bracket.
  • the glass window 111 may pass through the flange, the seal ring and the furnace cover 12, and the furnace body 11 is provided with a water cooling device 100 located on the side of the glass window 111 and used to cool the glass window 111.
  • the water cooling device 100 is a specific cooling process that takes away heat by flowing water, and the flowing water can be passed through the pipeline. Through the installation of the water-cooling device 100, the glass window 111 can be cooled to reduce the temperature of the glass window 111 and prevent the temperature of the glass window 111 from being too high to cause the problem of cracking.
  • the nano-material preparation device further includes a reaction gas input device 110.
  • the reaction gas input device 110 is connected to the reaction furnace 10 and is used to pass a reaction gas into the reaction furnace 10.
  • the reaction gas input device 110 is connected to the side of the furnace body 11 and sealed at the interface, so as to avoid the phenomenon of air leakage when the reaction gas is introduced into the furnace body 11 and ensure the preparation of nanometer powder. Reliability and stability.
  • the reaction gas passed into the furnace body 11 may be a gas such as methane, oxygen, or ammonia. Its role is to react the raw materials in the crucible 20 to form new required nano-materials during the process of melting, evaporating and cooling.
  • the nano-material preparation equipment further includes an alloy adding device 120, which is disposed in the reaction furnace 10 and is used for containing the alloy material and adding the alloy material to the crucible 20.
  • the alloy adding device 120 may add the alloy material contained therein to the crucible 20 and mix it with the original raw materials in the crucible 20, so that during the evaporation process, the alloy materials and the raw materials may form a chemical reaction to form alloy nano powders. body.
  • the alloy adding device 120 includes several material boxes for containing different alloy materials and for driving the material boxes (not shown) containing different alloy materials to open to add different alloy materials.
  • a driving element (not shown) from the alloy material to the crucible 20 is included in the alloy adding device 120.
  • the number of material boxes can be increased according to actual conditions. For example, thirteen material boxes can be provided. The thirteen material boxes can hold thirteen different alloy materials.
  • the driving element may be a motor, an air cylinder, or the like, or a motor, an air cylinder, or the like coupled with a transmission mechanism to control the material box to move and open.
  • the liquid phase capture device 70 includes a container 71, a gas collecting pipe 72, and a vacuum generator 73.
  • the container 71 is provided with a solution 711, and the reaction furnace 10 is provided with a gas collecting interface 112.
  • One end of the gas collection pipe 72 is connected to the gas collection interface 112, and the other end of the gas collection pipe 72 extends through the container 71 into the solution 711, and the vacuum generator 73 and the container 71 connections.
  • the container 71 is a double-layer stainless steel structure.
  • the container 71 is water-cooled in the middle.
  • the upper end of the gas collecting pipe 72 is connected to the gas collecting interface 112 provided on the furnace body 11 through a flange and a sealing ring.
  • the lower end extends through the container 71 to the container.
  • the gas collecting pipe 72 passes through the interface of the container 71 for sealing treatment.
  • a certain negative pressure is generated in the container 71 by the true vacuum generator 73, so that the nano-material in the furnace body 11 is drawn into the solution 711 in the container 71.
  • the nanomaterial can be cooled by the solution 711, but also the nanomaterial can be protected from passivation by the protection of the solution 711.
  • the solution 711 is preferably a non-volatile solution or a hardly volatile solution, and its function is to avoid affecting the operation of the vacuum generator 73.
  • the solution 711 may also be a solution that can be subsequently combined with the nanomaterial to form a specific product, for example, a solution that can be combined with the nanomaterial to form a conductive resin.
  • the liquid-phase capture device 70 further includes a thermocouple thermometer 74, and the thermocouple thermometer 74 is installed in the gas collection interface 112.
  • the thermocouple thermometer 74 is installed on the gas collection interface 112 to monitor the temperature of the nano-materials in the gas collection interface 112 in real time, so as to control the cooling gas flow from the cooling gas inlet device according to the temperature level. The amount of traffic.
  • the nano-material preparation equipment provided in this embodiment has at least the following advantages:
  • the temperature of induction melting and the temperature at which the laser is turned on can be controlled by infrared temperature measurement, which can avoid the separation of the alloy components or the improper composition ratio caused by the difference in element boiling point and vapor pressure during the evaporation process, and can also improve the evaporation efficiency;
  • the required powder can be directly collected into the required solution through the powder trapping device, which can prevent further growth of the nano-powder, shorten the production cycle, and reduce the production process.
  • a nanomaterial preparation device provided in this embodiment includes:
  • the crucible 20 is set in the reaction furnace 10 and used for containing raw materials
  • An evacuation device 30 connected to the reaction furnace 10 and configured to evacuate the inside of the reaction furnace 10;
  • a protective gas input device 40 which is connected to the reaction furnace 10 and is used to pass in a protective gas into the reaction furnace 10;
  • a magnetic levitation heating device 50 is disposed in the reaction furnace 10 and is located on the outer periphery of the crucible 20 and performs magnetic levitation heating on the raw materials in the crucible 20 until the raw materials are evaporated to form atom / molecular vapor;
  • the cooling gas input device 80 is connected to the reaction furnace 10, and the gas output end of the cooling gas input device 80 is directly opposite to the opening of the crucible 20 and is used to pass cooling gas to the suspension of the crucible 20. Said atomic / molecular vapor is cooled to form a nanomaterial;
  • the liquid-phase capture device 70 is connected to the reaction furnace 10 and is used to extract the nano-material into a liquid for further cooling.
  • this embodiment does not need to be provided with a laser heating device 60. It uses a magnetic suspension heating device 50 to perform magnetic suspension heating on the raw materials in the crucible 20 until the raw materials are made. Evaporates to form atomic / molecular vapors; suitable for processing low-boiling materials such as zinc or lead.
  • a method for preparing a nanomaterial provided in this embodiment includes the following steps:
  • the method for preparing a nano material according to the embodiment of the present invention may be specifically implemented by using the above-mentioned nano material preparation equipment.
  • the raw materials are suspended in the crucible 20 during heating and evaporation and separated from the crucible 20, thereby ensuring that the nanomaterials evaporated during the preparation process can still maintain their original Element ratio, there is no pollution source in the entire process of preparing nanomaterials, ensuring the production of high-purity nanomaterials; and, the evaporated nanomaterials are cooled by being extracted into the liquid to avoid further growth of the nanomaterials, eliminating the need for blunt nanomaterials It can reduce the number of production steps, shorten the production cycle, and finally collect the nanomaterials after further cooling.
  • the method may further include step S41: adding an alloy material to the crucible 20 and mixing and melting with the original material in the crucible 20, and finally evaporating the alloy nano-material.
  • Embodiment 4 Embodiment 4 .
  • a method for preparing a nanomaterial provided in this embodiment includes the following steps:
  • Cooling gas is passed to cool the atomic / molecular vapor suspended in the crucible 20 to form a nano material

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Abstract

一种纳米材料制备设备，包括反应炉(10)、坩埚(20)、抽真空装置(30)、保护气体输入装置(40)、位于坩埚的外周并对原料进行磁悬浮加热的磁悬浮加热装置(50)、设于反应炉外并用于发射激光对坩埚内的原料进行加热以使得原料蒸发形成原子/分子蒸气的激光加热装置(60)、与反应炉连接并用于通入冷却气体以对原子/分子蒸气进行冷却形成纳米材料的冷却气体输入装置(80)和与反应炉连接并抽取纳米材料进一步冷却的液相捕集装置(70)。以及一种纳米材料制备方法。采用上述纳米材料制备设备及方法可以避免对原料造成污染，保持高纯度，同时可以保证制备出的纳米粉体仍能保持其原来的元素比例。

Description

纳米材料制备设备和方法 技术领域
本发明属于纳米材料制备技术领域，尤其涉及一种纳米材料制备设备和方法。
 背景技术
把组成相或晶粒结构的尺寸控制在100nm以下的材料称为纳米材料，即将三维空间内至少有一维处在纳米尺度范围（1~100nm）的结构单元或由它们按一定规律构筑而成的材料或结构定义为纳米材料。纳米材料具有体积效应，表面效应，量子尺寸效应，量子隧道效应，介电限域效应，这些效应导致了纳米材料在熔点、蒸气压、光学性质、磁性、超导及塑性形变等许多物理和化学方面都显示出特殊的性能。这些特殊的性能使得纳米材料在电学、磁学、力学、催化和生物医疗等诸多领域称为一个新的研究热点。
目前纳米材料的制备多采用化学方法制备和物理方法，化学制备方法有化学气相反应法，化学气相沉积，沉淀法，水热法，溶胶-凝胶法，化学还原法。化学方法的缺点是制备过程中需要使用到溶剂，制备容易产生杂质，最后形成的纳米粉末容易聚集，难以分离，而且成球形性较差，制取纳米合金材料工艺复杂。物理制备方法有机械粉碎法，气相蒸发法，溅射法等。机械粉碎法制备纳米微粒的缺点是晶粒尺寸不均匀，易引入某些杂质。其中，采用气相蒸发法目前有电阻式加热，高频感应加热，电弧放电加热，激光加热，等离子加热。气相蒸发主要是采用一种加热方式，如电阻式加热和高频感应加热，这种方式比较难以制备高熔点低蒸气压物质，使用电弧放电加热方式缺点是容易产生微米量级大小的电极颗粒的飞溅，使用激光加热和等离子加热可以制取金属，合金或金属化合物纳米粒子，但是单纯的使用一种热源形式，耗能较高，而且对于低熔点高蒸气压的金属或者合金纳米制备过程中的工艺不好控制。对于物理蒸发法，大部分都会采用耐高温坩埚，在制备纳米材料的工艺中大部分纳米材料都需要在2000℃以上才会快速蒸发，这样高的温度就会造成有些材料与坩埚反应。同时，物理法制备的纳米粉末为干态，由于金属纳米粉末活性非常高，为了防止其直接暴露在空气中发生快速氧化而导致自燃，通常的做法是在收集前先通适当的氧气让合金材料表面进行钝化，但是这一过程时间耗时较长，而且表面钝化情况难以判断和控制。
目前越来越多科研学者将研究方向放在高纯纳米材料和合金纳米材料，而高纯纳米材料的制备不仅需要高纯的原料，还需要保证在制备过程中对原料无污染。制备合金纳米粉末时还需要保证合金纳米材料的成分比例不发生变化。所以针对如何避免在制备过程中带入污染，同时又保证能够在短时间内快速将材料蒸发，避免合金成分和比例的丢失这一问题，提出一种新型纳米材料制备设备和方法就显得尤为重要。
 技术问题
本申请实施例的目的在于：一方面，提供一种纳米材料制备设备，旨在解决制备高纯纳米材料过程中容易带来污染以及合金纳米材料制备过程中容易出现成分比例丢失的技术问题。
另一方面，提供一种纳米材料制备方法，旨在解决制备高纯纳米材料过程中容易带来污染以及合金纳米材料制备过程中容易出现成分比例丢失的技术问题。
 技术解决方案
为解决上述技术问题，本申请实施例采用的技术方案是：
提供了一种纳米材料制备设备，包括：
反应炉；
坩埚，设于所述反应炉内并用于盛放原料；
抽真空装置，与所述反应炉连接并用于对所述反应炉内进行抽真空；
保护气体输入装置，与所述反应炉连接并用于通入保护气体至所述反应炉内；
磁悬浮加热装置，设于所述反应炉内且位于所述坩埚的外周并对所述坩埚内的原料进行磁悬浮加热；
激光加热装置，设于所述反应炉外且其激光发射端正对所述反应炉设置并用于发射激光对所述坩埚内的原料进行加热以使得所述原料蒸发形成原子/分子蒸气；
冷却气体输入装置，与所述反应炉连接，且所述冷却气体输入装置的气体输出端正对所述坩埚的开口设置并用于通入冷却气体以对悬浮于所述坩埚内所述原子/分子蒸气进行冷却形成纳米材料；
液相捕集装置，与所述反应炉连接并用于抽取所述纳米材料至液体中进一步冷却。
提供了一种纳米材料制备设备，包括：
反应炉；
坩埚，设于所述反应炉内并用于盛放原料；
抽真空装置，与所述反应炉连接并用于对所述反应炉内进行抽真空；
保护气体输入装置，与所述反应炉连接并用于通入保护气体至所述反应炉内；
磁悬浮加热装置，设于所述反应炉内且位于所述坩埚的外周并对所述坩埚内的原料进行磁悬浮加热，并直至使得所述原料蒸发形成原子/分子蒸气；
冷却气体输入装置，与所述反应炉连接，且所述冷却气体输入装置的气体输出端正对所述坩埚的开口设置并用于通入冷却气体以对悬浮于所述坩埚内所述原子/分子蒸气进行冷却形成纳米材料；
液相捕集装置，与所述反应炉连接并用于抽取所述纳米材料至液体中进一步冷却。
为解决上述技术问题，本申请实施例采用的另一技术方案是：
提供了一种纳米材料制备方法，包括以下步骤：
S10：添加原料至反应炉内的坩埚中；
S20：对所述反应炉进行抽真空；
S30：通入保护气体至处于真空状态的所述反应炉内；
S40：对所述坩埚进行磁悬浮加热使得所述原料熔化悬浮于所述坩埚中；
S50：对悬浮于所述坩埚中的原料进行激光加热以使得所述原料蒸发形成原子/分子蒸气；
S60：通入冷却气体对悬浮于所述坩埚内所述原子/分子蒸气进行冷却形成纳米材料；
S70：抽取所述纳米材料至液体中进一步冷却。
提供了一种纳米材料制备方法，包括以下步骤：
S10：添加原料至反应炉内的坩埚中；
S20：对所述反应炉进行抽真空；
S30：通入保护气体至处于真空状态的所述反应炉内；
S40：对所述坩埚进行磁悬浮加热使得所述原料悬浮于所述坩埚中，并直至使得所述原料蒸发形成原子/分子蒸气；
S50：通入冷却气体对悬浮于所述坩埚内所述原子/分子蒸气进行冷却形成纳米材料；
S60：抽取所述纳米材料至液体中进一步冷却。
 有益效果
与现有技术相比，本申请的有益效果：本发明的纳米材料制备设备，具体操作时，先添加原料至反应炉内的坩埚中、接着通过抽真空装置对反应炉进行抽真空，接着通过保护气体输入装置通入保护气体至处于真空状态的反应炉内，接着通过磁悬浮加热装置对坩埚进行磁悬浮加热直至原料熔化悬浮于所述坩埚中，接着通过激光加热装置对悬浮于坩埚中的原料进行激光加热并直至使得原料蒸发原子/分子蒸气，冷却气体输入装置通入冷却气体以对悬浮于所述坩埚内原子/分子蒸气进行急速冷却形成纳米材料，最后液相捕集装置通过抽取纳米材料至液体中进一步冷却，并收集纳米材料。如此操作，原料在磁悬浮加热过程中悬浮于坩埚中而与坩埚分离不接触，以此保证整个制备过程中不存在污染源，确保制成高纯度的纳米材料；而且由于高能量的激光束可以在较短的时间内将物质的局部加热至极高的温度并产生物质的蒸发，在此过程中被蒸发出来的物质仍能保持其原来的元素比例；并且，蒸发出的纳米材料通过抽取至液体中冷却，避免纳米材料进一步长大，同时，省去对纳米材料钝化的工序，减少生产环节，缩短生产周期。
本发明的纳米材料制备方法，在制备过程中，原料的加热蒸发过程中悬浮于坩埚中而与坩埚分离不接触，以此保证制备过程中被蒸发的纳米材料能够仍然保持其原有的元素比例，整个制备纳米材料的过程中不存在污染源，确保制成高纯度的纳米材料；并且，蒸发出的纳米材料通过抽取至液体中冷却，避免纳米材料进一步长大，省去对纳米材料钝化的工序，减少生产环节，缩短生产周期。
 附图说明
为了更清楚地说明本发明实施例中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动性的前提下，还可以根据这些附图获得其他的附图。
图1为本发明实施例提供的纳米材料制备设备的结构示意图。
图2为本发明实施例三提供的纳米材料制备方法的流程图。
图3为本发明实施例四提供的纳米材料制备方法的流程图。
其中，图中各附图标记：
10—反应炉            11—炉体            12—炉盖
13—炉门              20—坩埚            30—抽真空装置
40—保护气体输入装置  50—磁悬浮加热装置  60—激光加热装置
70—液相捕集装置71—容器            72—集气管道
73—真空发生器        74—热电偶测温仪    80—冷却气体输入装置
90—红外测温装置      100—水冷装置       110—反应气体输入装置
111—玻璃窗           112—集气接口       113—激光进口
120—合金添加装置130—吹气装置       131—观察窗口
711—溶液。
 本发明的实施方式
下面详细描述本发明的实施例，所述实施例的示例在附图中示出，其中自始至终相同或类似的标号表示相同或类似的元件或具有相同或类似功能的元件。下面通过参考附图1~3描述的实施例是示例性的，旨在用于解释本发明，而不能理解为对本发明的限制。
在本发明的描述中，需要理解的是，术语“长度”、“宽度”、“上”、“下”、“前”、“后”、“左”、“右”、“竖直”、“水平”、“顶”、“底”“内”、“外”等指示的方位或位置关系为基于附图所示的方位或位置关系，仅是为了便于描述本发明和简化描述，而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本发明的限制。
此外，术语“第一”、“第二”仅用于描述目的，而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。由此，限定有“第一”、“第二”的特征可以明示或者隐含地包括一个或者更多个该特征。在本发明的描述中，“多个”的含义是两个或两个以上，除非另有明确具体的限定。
在本发明中，除非另有明确的规定和限定，术语“安装”、“相连”、“连接”、“固定”等术语应做广义理解，例如，可以是固定连接，也可以是可拆卸连接，或成一体；可以是机械连接，也可以是电连接；可以是直接相连，也可以通过中间媒介间接相连，可以是两个元件内部的连通或两个元件的相互作用关系。对于本领域的普通技术人员而言，可以根据具体情况理解上述术语在本发明中的具体含义。
实施例一。
如图1所示，本实施例提供的一种纳米材料制备设备，包括：
反应炉10，反应炉10作为可以实现封闭的结构，其为整个设备提供工作环境以及提供安装支撑。反应炉10能够在高温下工作，具有耐高温以及高密封性的优点。
坩埚20，设于所述反应炉10内并用于盛放原料，原料一般为金属粉体。其采用耐高温的材料制造形成。
抽真空装置30，与所述反应炉10连接并用于对所述反应炉10内进行抽真空。抽真空装置30与反应炉10的连接处做密封处理，以此避免因为接口处存在气密性问题而影响抽真空装置30的正常使用或者影响对反应炉10内的抽真空效果。抽真空装置30为一种可以实现对反应炉10内抽真空的装置，具体工作过程中通过产生负压而将反应炉10内原有的其他抽吸走，直至使得反应炉10内形成真空状态。
保护气体输入装置40，与所述反应炉10连接并用于通入保护气体至所述反应炉10内；保护气体输入装置40与反应炉10的连接处做密封处理，确保通入保护气体至反应炉10内时出现漏气。保护气体可以为氩气、氮气等。其中，氩气、氮气等保护气体的作用是用于保护坩埚20内的原料不发生氧化等其他质变，确保对原料的正常加热蒸发。
磁悬浮加热装置50，设于所述反应炉10内且位于所述坩埚20的外周并对所述坩埚20内的原料进行磁悬浮加热。磁悬浮加热装置50可以实现磁悬浮感应加热，一方面使得坩埚20内的原料处于悬浮于坩埚20中的状态，另一方面还能够对原料进行加热，使得原料加热至接近沸点以下的温度。
激光加热装置60，设于所述反应炉10外且激光加热装置60的激光发射端正对所述反应炉10设置并用于发射激光对所述坩埚20内的原料进行加热以使得所述原料蒸发形成原子/分子蒸气。激光加热装置60对悬浮于坩埚20中的原料进行加热，此时原料的温度在磁悬浮加热装置50的加热下接近沸点，那么经过激光加热装置60的进一步激光快速加热，激光加热装置60产生的高能量密度的激光原料的温度快速提升至沸点以上。
冷却气体输入装置80，与所述反应炉10连接，且所述冷却气体输入装置80的气体输出端正对所述坩埚20的开口设置并用于通入冷却气体以对悬浮于所述坩埚20内所述原子/分子蒸气进行冷却形成纳米材料。具体地，冷却气体输入装置80的气体输出端一般为管状结构，其延伸至坩埚20的上方即可。当悬浮于坩埚20内的原料在激光加热装置60的加热下温度达到沸点以上形成原子/分子蒸气，先通过冷却气体输入装置80通入冷却气体至炉体11对蒸发物质进行急速冷却，如此可以形成该物质的纳米材料。其中，通入的冷却气体可以是氮气、二氧化碳等冷却气体。
液相捕集装置70，与所述反应炉10连接并用于抽取所述纳米材料至液体中进一步冷却。蒸发出来的纳米材料经液相捕集装置70被快速抽取到液体中冷却，避免了纳米材料进一步的长大，同时也省去了钝化这一过程，最终实现收集。
以下对本实施例提供的纳米材料制备设备的操作作进一步说明，具体操作时，先添加原料至反应炉10内的坩埚20中、接着通过抽真空装置30对反应炉10进行抽真空，接着通过保护气体输入装置40通入保护气体至处于真空状态的反应炉10内，接着通过磁悬浮加热装置50对坩埚20进行磁悬浮加热直至原料熔化悬浮于所述坩埚20中，接着通过激光加热装置60对悬浮于坩埚20中的原料进行激光加热并直至使得原料蒸发形成原子/分子蒸气，冷却气体输入装置80通入冷却气体以对悬浮于所述坩埚20内原子/分子蒸气进行急速冷却形成纳米材料，最后液相捕集装置70通过抽取纳米材料至液体中进一步冷却，并收集纳米材料。如此操作，原料在磁悬浮加热过程中悬浮于坩埚20中而与坩埚20分离不接触，以此保证整个制备过程中不存在污染源，确保制成高纯度的纳米材料；而且由于高能量的激光束可以在较短的时间内将物质的局部加热至极高的温度并产生物质的蒸发，在此过程中被蒸发出来的物质仍能保持其原来的元素比例。并且，蒸发出的纳米材料通过抽取至液体中冷却，避免纳米材料进一步长大，同时，省去对纳米材料钝化的工序，减少生产环节，缩短生产周期。
优选地，坩埚20优选为水冷铜坩埚20。其一方面能够耐高温，另一方面其可以避免与原料发生化学反应，这样可以确保蒸发出的纳米材料具有高纯度，能够保持原有的元素比例。
当然，坩埚20还可以采用其他不与原料发生化学反应且具有高温性能的材料制造而成，在此不再一一列举赘述。
其中，磁悬浮加热装置50包括能够使得坩埚20中的原料处于悬浮状态的线圈，该线圈可以绕制在坩埚20的外壁上，并且该线圈还可以实现对原料进行加热的功能。
进一步地，磁悬浮加热装置50还可以包括专门实现对坩埚20内的原料进行加热的电阻或者其他加热元件，其可以辅助加热悬浮于坩埚20内的原料。
本实施例中，所述反应炉10包括炉体11、炉盖12和炉门13，所述炉体11的顶部和侧部分别设有顶开口（图未示）和侧开口（图未示），侧开口优选开设在纳米材料制备设备处于放置状态的前侧，以便于工作人员操作。所述炉盖12连接于所述炉体11的顶部并封盖于所述顶开口上，炉盖12与顶开口的一侧缘活动连接，这样便于开启炉盖12，并且关闭炉盖12后能够完全密封住顶开口。同样，所述炉门13连接于所述炉体11的侧部并封盖于所述侧开口上，炉门13与侧开口的一侧缘活动连接，这样便于开启炉门13，并且关闭炉门13后能够完全封盖于侧开口。
其中，开启炉盖12可以便于安装各种位于炉体11的装置，及对各装置进行检修和维护。而开启炉门13则可以便于添加原料至坩埚20内。
优选地，保护气体输入装置40、磁悬浮加热装置50和液相捕集装置70连接于炉体11的侧部，而激光加热装置60则设置在炉盖12的上方。进一步地，所述反应炉10的炉盖12上设有激光进口113，所述激光加热装置60的激光发射端正对所述激光进口113设置。具体地，激光进口113的设置用于供设置在炉盖12上方的激光加热装置60发射出的激光通过，通过激光进口113的激光可以对悬浮于坩埚20中的原料进行进一步的加热，直至使得原料的温度达到沸点以上并蒸发。
进一步地，所述反应炉10内位于所述激光进口113的侧方设有用于朝向所述激光进口113吹气以防止粉末聚集在所述激光进口113的吹气装置130。吹气装置130的设置可以对激光进口113处吹出气体，这样可以避免炉体11内的粉末剧集在该激光进口113处阻挡住激光的通过，提升激光加热装置60使用的稳定性和可靠性。其中，吹气装置130可以是风机。
进一步地，所述炉门13上设有观察窗口131。观察窗口131为透明窗口，其作用是供工作人员在制备全过程可以通过观察窗口131观察监视炉体11内的状态，以判断制备纳米粉体过程中的原料的变化状态。
其中，炉体11为双层不锈钢结构，内层有冷却结构。炉盖12为双层不锈钢结构，内层有冷却结构，炉门13为双层不锈钢结构，内层有冷却结构。
进一步地，冷却气体输入装置80与反应炉10的炉体11的侧部连接，且接口处作密封处理，避免通入冷却气体至反应炉10内时出现漏气的现象。
本实施例中，所述纳米材料制备设备还包括红外测温装置90，所述红外测温装置90设于所述反应炉10之外，所述反应炉10上设有供所述红外测温装置90投射的红外线通过以探测所述坩埚20内的材料的温度的玻璃窗111，玻璃窗111优选设置在炉盖12上。具体地，红外测温装置90可以发射红外线通过设置在炉盖12上的玻璃窗111投射到坩埚20内，对坩埚20内的原料的温度进行实时监测，根据材料蒸发温度将磁悬浮加热装置50感应加热时对坩埚20内的材料的温度控制在合理范围内，防止原料中某些低沸点高蒸气压的成分先行蒸发，造成合金粉末的成分比例失调，其主要与磁悬浮加热装置50配合使用。
进一步地，红外测温装置90可以通过固定支架与炉盖12相连。
进一步地，玻璃窗111可以通过法兰盘、密封圈与炉盖12，并且在所述炉体11上设有位于所述玻璃窗111的侧方并用于冷却所述玻璃窗111的水冷装置100，水冷装置100是具体冷却过程为通过流动的水将热量带走，流动的水可以通过管道实现通过。通过水冷装置100的设置，可以对玻璃窗111进行降温，起到给玻璃窗111降温的作用，防止玻璃窗111的温度过高而出现炸裂的问题。
本实施例中，所述纳米材料制备设备还包括反应气体输入装置110，所述反应气体输入装置110与所述反应炉10连接并用于通入反应气体至所述反应炉10内。其中，反应气体输入装置110与炉体11的侧部连接，并且在接口出作密封处理，以此避免在通入反应气体至炉体11内时出现漏气的现象，保证制备纳米粉体的可靠性和稳定性。通入炉体11内的反应气体可以是甲烷、氧气、氨气等气体。其作用是坩埚20内的原料在熔化蒸发冷却过程中反应形成新的所需的纳米材料。
进一步地，所述纳米材料制备设备还包括合金添加装置120，所述合金添加装置120设于所述反应炉10内并用于盛装合金材料以及添加所述合金材料至所述坩埚20内。具体地，合金添加装置120可以将其内盛装的合金材料添加至坩埚20中，与坩埚20中原有的原料混合，这样在蒸发过程中，可以使得合金材料与原料形成化学反应从而形成合金纳米粉体。
本实施例中，所述合金添加装置120包括若干个用于盛装不同合金材料的材料盒以及用于驱动盛装有不同的所述合金材料的所述材料盒（图未示）开启以添加不同的所述合金材料至所述坩埚20内的驱动元件（图未示）。具体地，材料盒的数量可以根据实际情况增加，例如可以设置十三个材料盒，通过十三个材料盒可以盛装十三种不同的合金材料，需要具体添加哪种合金材料时，可以通过驱动元件驱动该种材料盒移动并开启，以此实现将合金材料添加至坩埚20中。驱动元件可以是电机、气缸等或者通过电机、气缸等配合传动机构以控制材料盒移动并且开启。
本实施例中，所述液相捕集装置70包括容器71、集气管道72和真空发生器73，所述容器71内设有溶液711，所述反应炉10上设有集气接口112，所述集气管道72的一端与所述集气接口112连接，所述集气管道72的另一端穿过所述容器71伸入所述溶液711内，所述真空发生器73与所述容器71连接。具体地，容器71为双层不锈钢结构，容器71中间通水冷，集气管道72的上端通过法兰和密封圈与炉体11上设置的集气接口112相连，下端穿过容器71伸入容器71内的溶液711内，其中集气管道72穿过容器71的接口处作密封处理。工作时，通过真真空发生器73使得容器71内产生一定负压，从而使得炉体11内的纳米材料抽向容器71内的溶液711中。如此，不但可以通过溶液711对纳米材料进行冷却，还可以通过溶液711的保护避免纳米材料钝化。
溶液711优选为非挥发性溶液或者难以挥发的溶液，其作用是避免影响真空发生器73的工作。
另外，该溶液711还可以采用后续可以与纳米材料结合形成特定产品的溶液，例如可以与纳米材料结合形成导电树脂的溶液。
本实施例中，所述液相捕集装置70还包括热电偶测温仪74，所述热电偶测温仪74安装于所述集气接口112中。具体地，热电偶测温仪74安装在集气接口112，实时监测纳米材料缓和有的气体在集气接口112中的温度，从而根据温度的高低控制冷却气体通入装置通入的冷却气体的流量的大小。
综上所述，本实施例提供的纳米材料制备设备至少具有以下优点：
一，通过磁悬浮感应熔炼技术，避免了高温情况下原料与坩埚20反应，造成材料的污染，可以制备高纯纳米粉末；
二，通过红外测温控制感应熔炼的温度和激光开启的温度，可以避免在蒸发过程中由于元素沸点和蒸气压的区别造成的合金成分的分离或者是成分比例失调，同时还能提高蒸发效率；
三，通过粉体捕集装置可以直接将所需粉体收集到所需溶液中，可以阻止纳米粉末进一步的长大，缩短了生产周期，减少了生产环节。
实施例二。
如图1所示，本实施例提供的一种纳米材料制备设备，其包括：
反应炉10；
坩埚20，设于所述反应炉10内并用于盛放原料；
抽真空装置30，与所述反应炉10连接并用于对所述反应炉10内进行抽真空；
保护气体输入装置40，与所述反应炉10连接并用于通入保护气体至所述反应炉10内；
磁悬浮加热装置50，设于所述反应炉10内且位于所述坩埚20的外周并对所述坩埚20内的原料进行磁悬浮加热，并直至使得所述原料蒸发形成原子/分子蒸气；
冷却气体输入装置80，与所述反应炉10连接，且所述冷却气体输入装置80的气体输出端正对所述坩埚20的开口设置并用于通入冷却气体以对悬浮于所述坩埚20内所述原子/分子蒸气进行冷却形成纳米材料；
液相捕集装置70，与所述反应炉10连接并用于抽取所述纳米材料至液体中进一步冷却。
本实施例与上述实施例一的不同之处在于：本实施例不在需要设置激光加热装置60，其通过磁悬浮加热装置50，对所述坩埚20内的原料进行磁悬浮加热，并直至使得所述原料蒸发形成原子/分子蒸气；适用于沸点较低的原料进行加工，例如锌或者铅等。
本实施例的其余部分与实施例一相同，其技术效果同上述实施例一相同，在本实施例中未解释的特征，均采用实施例一的解释，这里不再进行赘述。
实施例三。
如图1和2所示，本实施例提供的一种纳米材料制备方法，其包括以下步骤：
S10：添加原料至反应炉10内的坩埚20中；
S20：对所述反应炉10进行抽真空；
S30：通入保护气体至处于真空状态的所述反应炉10内；
S40：对所述坩埚20进行磁悬浮加热使得所述原料熔化悬浮于所述坩埚20中；
S50：对悬浮于所述坩埚20中的原料进行激光加热以使得所述原料蒸发形成原子/分子蒸气；
S60：通入冷却气体对悬浮于所述坩埚20内所述原子/分子蒸气进行冷却形成纳米材料；
S70：抽取所述纳米材料至液体中进一步冷却。
本发明实施例的纳米材料制备方法，具体可以采用上述的纳米材料制备设备进行操作实现。在采用该制备方法制备纳米材料的过程中，原料的加热蒸发过程中悬浮于坩埚20中而与坩埚20分离不接触，以此保证制备过程中被蒸发出的纳米材料能够仍然保持其原有的元素比例，整个制备纳米材料的过程中不存在污染源，确保制成高纯度的纳米材料；并且，蒸发出的纳米材料通过抽取至液体中冷却，避免纳米材料进一步长大，省去对纳米材料钝化的工序，减少生产环节，缩短生产周期，最后可以收集进一步冷却后的纳米材料。
进一步地，在步骤S40之后，步骤S50之前还可以包括步骤S41：添加合金材料至坩埚20中与坩埚20中原有的材料混合熔炼，最后蒸发出合金纳米材料。
实施例四。
如图1和3所示，本实施例提供的一种纳米材料制备方法，包括以下步骤：
S10：添加原料至反应炉10内的坩埚20中；
S20：对所述反应炉10进行抽真空；
S30：通入保护气体至处于真空状态的所述反应炉20内；
S40：对所述坩埚20进行磁悬浮加热使得所述原料熔化悬浮于所述坩埚20中，并直至使得所述原料蒸发形成原子/分子蒸气；
S50：通入冷却气体对悬浮于所述坩埚20内所述原子/分子蒸气进行冷却形成纳米材料；
S60：抽取所述纳米材料至液体中进一步冷却。
本实施例与实施例三的区别之处在于：本实施例不在需要进行激光加热，其对所述坩埚内的原料进行磁悬浮加热，并直至使得所述原料蒸发形成原子/分子蒸气；适用于沸点较低的原料进行加工，例如锌或者铅等。
本实施例的其余部分与实施例一相同，其技术效果同上述实施例一相同，在本实施例中未解释的特征，均采用实施例一的解释，这里不再进行赘述。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (16)

  1. 一种纳米材料制备设备，其特征在于：包括：
    反应炉；
    坩埚，设于所述反应炉内并用于盛放原料；
    抽真空装置，与所述反应炉连接并用于对所述反应炉内进行抽真空；
    保护气体输入装置，与所述反应炉连接并用于通入保护气体至所述反应炉内；
    磁悬浮加热装置，设于所述反应炉内且位于所述坩埚的外周并对所述坩埚内的原料进行磁悬浮加热；
    激光加热装置，设于所述反应炉外且其激光发射端正对所述反应炉设置并用于发射激光对所述坩埚内的原料进行加热以使得所述原料蒸发形成原子/分子蒸气；
    冷却气体输入装置，与所述反应炉连接，且所述冷却气体输入装置的气体输出端正对所述坩埚的开口设置并用于通入冷却气体以对悬浮于所述坩埚内所述原子/分子蒸气进行冷却形成纳米材料；
    液相捕集装置，与所述反应炉连接并用于抽取所述纳米材料至液体中进一步冷却并保存。
  2. 一种纳米材料制备设备，其特征在于：包括：
    反应炉；
    坩埚，设于所述反应炉内并用于盛放原料；
    抽真空装置，与所述反应炉连接并用于对所述反应炉内进行抽真空；
    保护气体输入装置，与所述反应炉连接并用于通入保护气体至所述反应炉内；
    磁悬浮加热装置，设于所述反应炉内且位于所述坩埚的外周并对所述坩埚内的原料进行磁悬浮加热，并直至使得所述原料蒸发形成原子/分子蒸气；
    冷却气体输入装置，与所述反应炉连接，且所述冷却气体输入装置的气体输出端正对所述坩埚的开口并用于通入冷却气体以对悬浮于所述坩埚内所述原子/分子蒸气进行快速冷却形成纳米材料；
    液相捕集装置，与所述反应炉连接并用于抽取所述纳米材料至液体中进一步冷却和收集。
  3. 根据权利要求1或2所述的纳米材料制备设备，其特征在于：所述纳米材料制备设备还包括红外测温装置，所述红外测温装置设于所述反应炉之外，所述反应炉上设有供所述红外测温装置投射的红外线通过以探测所述坩埚内的材料的温度的玻璃窗。
  4. 根据权利要求3所述的纳米材料制备设备，其特征在于：所述炉体上设有位于所述玻璃窗的侧方并用于冷却所述玻璃窗的水冷装置。
  5. 根据权利要求1或2所述的纳米材料制备设备，其特征在于：所述纳米材料制备设备还包括反应气体输入装置，所述反应气体输入装置与所述反应炉连接并用于通入反应气体至所述反应炉内。
  6. 根据权利要求1或2所述的纳米材料制备设备，其特征在于：所述纳米材料制备设备还包括合金添加装置，所述合金添加装置设于所述反应炉内并用于盛装合金材料以及添加所述合金材料至所述坩埚内。
  7. 根据权利要求6所述的纳米材料制备设备，其特征在于：所述合金添加装置包括若干个用于盛装不同合金材料的材料盒以及用于驱动盛装有不同的所述合金材料的所述材料盒开启以添加不同的所述合金材料至所述坩埚内的驱动元件。
  8. 根据权利要求1或2所述的纳米材料制备设备，其特征在于：所述液相捕集装置包括容器、集气管道和真空发生器，所述容器内设有溶液，所述反应炉上设有集气接口，所述集气管道的一端与所述集气接口连接，所述集气管道的另一端穿过所述容器伸入所述溶液内，所述真空发生器与所述容器连接。
  9. 根据权利要求8所述的纳米材料制备设备，其特征在于：所述液相捕集装置还包括热电偶测温仪，所述热电偶测温仪安装于所述集气接口中。
  10. 根据权利要求1或2所述的纳米材料制备设备，其特征在于：所述反应炉上设有激光进口，所述激光加热装置的激光发射端正对所述激光进口装置。
  11. 根据权利要求10所述的纳米材料制备设备，其特征在于：所述反应炉内位于所述激光进口的侧方设有用于朝向所述激光进口吹气以防止粉末聚集在所述激光进口的吹气装置。
  12. 根据权利要求1或2所述的纳米材料制备设备，其特征在于：所述反应炉包括炉体、炉盖和炉门，所述炉体的顶部和侧部分别设有顶开口和侧开口，所述炉盖连接于所述炉体的顶部并封盖于所述顶开口上，所述炉门连接于所述炉体的侧部并封盖于所述侧开口上。
  13. 根据权利要求12所述的纳米材料制备设备，其特征在于：所述炉门上设有观察窗口。
  14. 根据权利要求1或2所述的纳米材料制备设备，其特征在于：所述坩埚为水冷铜坩埚。
  15. 一种纳米材料制备方法，其特征在于：包括以下步骤：
    S10：添加原料至反应炉内的坩埚中；
    S20：对所述反应炉进行抽真空；
    S30：通入保护气体至处于真空状态的所述反应炉内；
    S40：对所述坩埚进行磁悬浮加热使得所述原料熔化悬浮于所述坩埚中；
    S50：对悬浮于所述坩埚中的原料进行激光加热以使得所述原料蒸发形成原子/分子蒸气；
    S60：通入冷却气体对悬浮于所述坩埚内所述原子/分子蒸气进行冷却形成纳米材料；
    S70：抽取所述纳米材料至液体中进一步冷却。
  16. 一种纳米材料制备方法，其特征在于：包括以下步骤：
    S10：添加原料至反应炉内的坩埚中；
    S20：对所述反应炉进行抽真空；
    S30：通入保护气体至处于真空状态的所述反应炉内；
    S40：对所述坩埚进行磁悬浮加热使得所述原料熔化悬浮于所述坩埚中，并直至使得所述原料蒸发形成原子/分子蒸气；
    S50：通入冷却气体对悬浮于所述坩埚内所述原子/分子蒸气进行冷却形成纳米材料；
    S60：抽取所述纳米材料至液体中进一步冷却。
PCT/CN2018/100442 2018-08-14 2018-08-14 纳米材料制备设备和方法 WO2020034090A1 (zh)

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CN102950293A (zh) * 2012-10-15 2013-03-06 宁波广博纳米新材料股份有限公司 纳米铝粉的生产方法
JP5750681B2 (ja) * 2014-02-12 2015-07-22 株式会社新光化学工業所 多元金属ナノ粒子コロイド、多元金属ナノ粒子コロイドの製造方法および金属ナノ粒子及び／又は多元金属ナノ粒子を担持した状態の担体
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CN1382547A (zh) * 2002-02-08 2002-12-04 宁波广博纳米材料有限公司 生产纳米金属粉装置
CN101015861A (zh) * 2006-11-09 2007-08-15 昆山密友实业有限公司 纳米金属粉体连续生产设备
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