CN218673102U - Spiral feeding tube furnace system for preparing two-dimensional material - Google Patents

Spiral feeding tube furnace system for preparing two-dimensional material Download PDF

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Publication number
CN218673102U
CN218673102U CN202222984715.8U CN202222984715U CN218673102U CN 218673102 U CN218673102 U CN 218673102U CN 202222984715 U CN202222984715 U CN 202222984715U CN 218673102 U CN218673102 U CN 218673102U
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furnace
tube
furnace tube
spiral
spiral feeding
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杨树斌
杜志国
杨运洋
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Jinan Sanchuan New Material Technology Co ltd
Beihang University
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Jinan Sanchuan New Material Technology Co ltd
Beihang University
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Abstract

The utility model discloses a spiral feeding tube furnace system for preparing two-dimensional materials, which comprises a furnace tube, a feeder, a rotating motor, a spiral feeding rod, a first heating system, a second heating system and a product collecting device; the feeder is connected with the furnace tube and is used for feeding the powder material into the furnace tube; the furnace tube comprises a reaction chamber and a product collection chamber; the rotary motor is connected with the spiral feeding rod, and the powder materials are driven to move in the furnace tube through the rotation of the spiral feeding rod and sequentially pass through the reaction chamber and the product collecting chamber; a first heating system surrounds the reaction chamber and a second heating system surrounds the product collection chamber; the product collecting device is connected with the product collecting chamber and is used for collecting the powder pushed by the spiral feeding rod. The utility model discloses avoided a large amount of precursors to pile up in tubular furnace hearth and leaded to reacting insufficient difficult problem, realized continuous reaction and collection, also can realize the scale continuous preparation of two-dimensional material.

Description

Spiral feeding tube furnace system for preparing two-dimensional material
Technical Field
The utility model relates to a two-dimensional material field especially relates to a spiral feeding tube furnace system of preparation two-dimensional material.
Background
Two-dimensional materials, such as MXene, transition metal chalcogenides (MoS), are currently prepared 2 、MoSe 2 And the like), placing a precursor material at the central position of a hearth of the tubular furnace, introducing inert gas to heat the precursor material, and introducing reactive gas to react to prepare the two-dimensional material after the reaction temperature is reached. And after the reaction is finished, stopping heating the tubular furnace, and taking out the two-dimensional material to finish the whole preparation process of the two-dimensional material.
However, the preparation of two-dimensional materials using a tube furnace has the following problems: firstly, a large amount of precursor materials are accumulated in a hearth of a tubular furnace and are in insufficient contact with reactive gases, so that the reaction is insufficient and is difficult to carry out complete reaction, and therefore, the preparation of two-dimensional materials by using the tubular furnace is only limited to research and development levels and is difficult to carry out large-scale preparation; secondly, the reactive gas reacts with the raw material precursor to prepare the two-dimensional material, a large amount of intermediate is generated, the intermediate is condensed at the tail end of the tube furnace, the tube furnace is blocked, potential safety hazards of explosion are brought, the intermediate is condensed on the tube wall of the tube furnace and is difficult to effectively collect, and the intermediate is easy to mix with the prepared two-dimensional material during sampling, so that the two-dimensional material contains a large amount of impurities; and thirdly, the two-dimensional material is prepared by adopting the tube furnace, only a single reaction can be carried out, and after the reaction is finished, the tube furnace needs to be cleaned and dried, so that the large-scale continuous preparation of the two-dimensional material is difficult to realize.
SUMMERY OF THE UTILITY MODEL
In view of the above, it is necessary to provide a spiral feeding tube furnace system capable of continuously preparing two-dimensional materials with high purity on a large scale.
The utility model provides a spiral feeding tube furnace system for preparing two-dimensional materials, which comprises a furnace tube, a feeder, a rotating motor, a spiral feeding rod, a first heating system, a second heating system and a product collecting device; the feeder is connected with the furnace tube and is used for feeding the powder material into the furnace tube; the furnace tube comprises a reaction chamber and a product collection chamber; the rotary motor is connected with the spiral feeding rod, and the rotation of the spiral feeding rod drives the powder material to move in the furnace tube and sequentially pass through the reaction chamber and the product collecting chamber; a first heating system surrounds the reaction chamber and a second heating system surrounds the product collection chamber; the product collecting device is connected with the product collecting chamber and is used for collecting the powder pushed by the spiral feeding rod.
In some embodiments, the furnace tube comprises: connecting the furnace tube, the first heating zone furnace tube and the second heating zone furnace tube; the connecting furnace tube is connected with the feeder, the first heating system surrounds the first heating zone furnace tube, and the interior of the first heating zone furnace tube is defined as the reaction chamber; the second heating system surrounds the second heating zone furnace, the interior of the second heating zone furnace being defined as the product collection chamber.
In some embodiments, a plurality of product discharge ports are disposed in the product collection chamber and are respectively connected to the storage tanks of the product collection device.
In some embodiments, the connecting piping of each of the product outlets to the storage tank is provided with an outlet flapper valve.
In some embodiments, a vent is provided on the connecting pipe of each product outlet and the storage tank for evacuating and/or introducing a protective gas into the storage tank.
In some embodiments, the furnace tube has a first end and a second end opposite to each other, the first end is connected with the gas inlet device, and the second end is connected with the gas outlet; the air inlet device is provided with a first air inlet and a second air inlet, the first air inlet is used for being connected with a vacuumizing device, and the second air inlet is used for being connected with a protective gas supply device.
In some embodiments, a rotary bearing is disposed in the furnace tube, and is used for fixedly supporting the spiral feeding rod to realize rotation of the spiral feeding rod.
In some embodiments, the rotary bearing is disposed at an end adjacent to the air outlet.
In some embodiments, the spiral feed tube furnace system comprises a sealed magnetic fluid flange and/or a plurality of adapter flanges.
In some embodiments, the rotating motor and the spiral feeding rod form a spiral feeding device, and the sealing magnetic fluid flange is used to connect the furnace tube and the spiral feeding device, so as to achieve the sealing effect under the rotation condition of the spiral feeding rod.
In some embodiments, the plurality of adapter flanges are used for assembling and connecting furnace tube components, and have connecting and sealing functions.
In some embodiments, the feeder is capable of continuously feeding the reaction raw material powder into the furnace tube for a predetermined period of time, so as to achieve continuous preparation.
In some embodiments, the first heating system and the second heating system are the same heating device.
Compared with the prior art, the utility model provides a preparation two-dimensional material's spiral feeding tube furnace system and application method thereof has following advantage:
firstly, a spiral feeding tube furnace system is adopted to prepare a two-dimensional material, so that the problem of insufficient reaction caused by accumulation of a large amount of precursor materials in a furnace chamber of a tube furnace is solved, and the large-scale preparation of the two-dimensional material is realized;
secondly, directional collection of products for preparing the two-dimensional material is realized, potential explosion safety hazards caused by condensation of an intermediate at the tail end of the tube furnace are avoided, and the prepared two-dimensional material has high purity;
third, the utility model discloses a spiral feeding tube furnace system has included feeder and result collection device preparation two-dimensional material, can realize continuous reaction and collection, has also realized the scale continuous preparation of two-dimensional material.
Drawings
Fig. 1 is a schematic structural diagram of a spiral-feeding tube furnace system for preparing two-dimensional materials according to an embodiment of the present invention.
Fig. 2 is a schematic structural diagram of a spiral feeding tube furnace system for preparing two-dimensional materials according to an embodiment of the present invention.
Fig. 3 is a schematic structural diagram of a spiral feeding tube furnace system for preparing two-dimensional materials according to a third embodiment of the present invention.
FIG. 4 shows MXene Ti of 10 kg level prepared by the spiral feeding tube furnace system of embodiment 1 of the present invention 3 C 2 Cl x An optical photograph of (a).
FIG. 5 shows that the MAX phase material provided in embodiment 1 of the present invention is Ti 3 AlC 2 (a) And MXene Ti as target product prepared by spiral feeding tube furnace system 3 C 2 Cl x (b) Scanning Electron Microscope (SEM) photograph of (a).
FIG. 6 shows that the MAX phase material provided in embodiment 1 of the present invention is Ti 3 AlC 2 And MXene Ti as target product prepared by spiral feeding tube furnace system 3 C 2 Cl x X-ray diffraction (XRD) pattern of (a).
FIG. 7 shows MXene Ti prepared in a conventional tube furnace as provided in comparative example 1 of the present invention 3 C 2 Cl x XRD pattern of (a).
Description of the main reference numerals:
100. 200, 300-spiral feed tube furnace system;
10-furnace tube; 11-a first connecting furnace tube; 12-a first heating zone furnace tube; 13-a second heating zone furnace tube; 14-a second connecting furnace tube; 101-a first end; 102-a second end; 103-gas outlet;
20-a feeder; 21-a storage container; 22-connecting tube; 221-a gas valve; 23-a flapper valve; 24-pressure gauge;
30-a rotating electrical machine;
40-a screw feed rod; 41-a rotational bearing;
51-a first heating system; 52-a second heating system;
60-a product collection device; 61-a storage tank; 62-a storage tank; 63-a first discharge flapper valve; 64-a second discharge flapper valve; 65-connecting port; 651-vent valve; 66-connecting port; 661-vent valve;
70-an air intake device; 71-a first vent; 711-a vent valve; 72-a second vent; 721-a vent valve; 73-a third vent; 731-pressure gauge;
81-sealing the magnetofluid flange; 82-a transfer flange; 83-a transfer flange; 84-sealing flange; 85-adapter flange;
90-a byproduct collection device; 91-a byproduct storage tank; 92-a third discharge flapper valve; 93-connection port; 931-a vent valve; 94-a vent valve; 95-a vent valve; 96-a storage container; 961-exhaust valve; 97-cooling means.
Detailed Description
The technical solution of the present invention is explained below by specific examples. It is to be understood that one or more steps recited herein are not exclusive of other methods or steps being present before or after the step of combining or intervening between those explicitly recited steps. It should also be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Unless otherwise indicated, the numbering of the various method steps is only for the purpose of identifying the various method steps, and is not intended to limit the scope of the invention, which may be practiced without substantial technical change, by changing or adjusting the relative relationship between the method steps.
The utility model discloses a two-dimensional material that spiral feeding tube furnace system is applicable to the preparation includes: MXene materials and/or two-dimensional transition metal chalcogenides (TDMs), both of which can be reacted in the gas phase and in the solid phase to give two-dimensional materials.
One of the MXene materials can be reacted with MAX phase materials through a gas phase etchant to etch the component A, so that an MXene material with an accordion appearance is obtained, the obtained MXene material with the accordion appearance can be subjected to a further stripping step to obtain a two-dimensional flaky MXene material, and the implementation mode of small-scale preparation by adopting a conventional tube furnace is described in the applicant's prior patent application ' method and system for preparing a two-dimensional material by a gas phase method ' (application number: 202011466046.4);
one of the transition metal chalcogenide compounds can be prepared by performing topological transformation reaction on a chalcogenide or phosphorus group gas and a MAX phase material to obtain a two-dimensional transition metal chalcogenide compound with an accordion shape or an expanded shape, and a two-dimensional sheet transition metal chalcogenide material can be obtained by further stripping, and the implementation mode and topological transformation synthesis raw materials prepared in a conventional tube furnace in a small scale are described in the prior patent applications of the applicant, namely a preparation method of the expanded transition metal chalcogenide compound (application number: 201811080797.5) and a synthesis method of the two-dimensional transition metal chalcogenide compound (application number: 201910995184.2).
The applicant summarizes the characteristics and the problems of the two types of two-dimensional material preparation processes, and provides equipment capable of preparing the two-dimensional material in a large scale and a using method of the equipment; the utility model discloses an equipment still can be applicable to other scenes that exist gas and solid powder reaction.
The spiral feeding tube furnace system for preparing two-dimensional materials and the use method thereof provided by the utility model are further explained with the attached drawings.
Example one
Referring to fig. 1, a first embodiment of the present invention provides a spiral-feeding tube furnace system 100 for preparing two-dimensional materials, which includes a furnace tube 10, a feeder 20, a rotary motor 30, a spiral-feeding rod 40, a first heating system 51, a second heating system 52, and a product collecting device 60. Wherein, boiler tube 10 cover is located inside the furnace body of spiral feeding tube furnace system, in this embodiment, boiler tube 10 passes through each partial pipe fitting of flange joint and constitutes, includes: a first connecting furnace tube 11, a first heating zone furnace tube 12, a second heating zone furnace tube 13; the first connecting furnace tube 11 is used for connecting an external device or equipment, and in this embodiment, a connecting port is formed in the first connecting tube and is communicated with the storage container 21 of the feeder 20, so that the reaction raw material powder in the feeder 20 enters the furnace tube 10; the first heating zone furnace tube 12 has a reaction chamber (a two-dimensional material preparation process, i.e., a gas-phase and solid-phase reaction process, occurs in the reaction chamber), and the second heating zone furnace tube 13 has a product collection chamber.
In the present embodiment, the first connecting furnace tube 11, the first heating zone furnace tube 12, and the second heating zone furnace tube 13 are connected together by the adapter flanges 82, 83, respectively; it is understood that in other embodiments, the first connecting furnace 11, the first heating zone furnace 12, and the second heating zone furnace 13 may be integrally formed furnaces; alternatively, the first heating zone furnace tube 12 and the second heating zone furnace tube 13 are integrally formed furnace tubes, that is, the first heating zone furnace tube 12 and the second heating zone furnace tube 13 are designed as two zones of one furnace tube.
In other embodiments, the furnace tube of the present invention may further include a connecting tube to communicate with other devices or apparatuses, and to connect the inside of the furnace tube with an external component to perform a specific function, such as adding or removing materials.
The first connecting furnace 11 and the second heating zone furnace 13 are preferably made of metal materials that are easy to mold, and in this embodiment, the first connecting furnace 11 and the second heating zone furnace 13 are made of stainless steel materials. The first heating zone furnace tube 12 is made of a high temperature resistant and corrosion resistant material, including a quartz tube, a corundum tube, a ceramic tube, a graphite tube, etc., and in this embodiment, a quartz tube is selected.
The storage container 21 of the feeder 20 is connected to the first connecting furnace 11 through a communicating pipe, a baffle valve 23 is disposed between the communicating pipes, and the feeder 20 is controlled to be connected to or separated from the chamber of the furnace 10, so as to control the powder material to enter or stop entering the furnace 10, or control the gas to enter or exit the furnace 10. In this embodiment, a connection pipe 22 is further connected to the connection pipe for connecting a vacuum pump or a protective gas (such as argon) supply device, and a gas valve 221 is disposed on the connection pipe for controlling the opening or closing of the connection pipe 22. The communicating pipe is also provided with a pressure gauge 24 for monitoring the pressure inside the feeder 20 in real time. In this embodiment, the connection tube 22 is connected to a vacuum pump (not shown) for vacuum pumping; in another embodiment, the connection pipe 22 can also be connected to a protective gas supply device to introduce a protective gas into the feeder 20 or the furnace tube 10. In a preferred embodiment, the feeder 20 is an automatic feeder, which can continuously supply powder material to the furnace tube 10, so that the spiral-feeding tube furnace system 100 of the present invention can realize continuous production.
The rotating motor 30 is connected with the spiral feeding rod 40 to rotate the spiral feeding rod 40, and the spiral feeding rod 40 penetrates through the furnace tube 10. The spiral feeding rod 40 can push the powder material in the furnace tube 10 by rotation, so that the powder material continuously advances, the powder material and the reaction gas realize reaction in the process that the powder material advances through the reaction chamber of the first heating zone furnace tube 12, the advancing speed range of the spiral feeding rod 40 is 0.01cm/min to 100cm/min, and the retention time of the material in the reaction chamber can be controlled by the advancing speed. The rotary motor 30 and the spiral feeding rod 40 form a spiral feeding device.
The residence time of the powder material in the first heating zone furnace tube 12 and the second heating zone furnace tube 13 can be controlled by designing the lengths of the first heating zone furnace tube 12 and the second heating zone furnace tube 13 and the rotation speed of the spiral feeding rod 40. In some embodiments, optionally, the first and/or second furnace zone 12, 13 can have a length between 0.5m and 20m.
The furnace tube 10 has opposite first and second ends 101 and 102, the first end 101 is communicated with the gas inlet device 70, and the second end 102 is communicated with the gas outlet 103 through the sealing flange 84; in this embodiment, the first end 101 is the end of the first connecting furnace tube 11, and is connected to the spiral feeding device through the sealing magnetic fluid flange 81, and the second end is provided with a rotary bearing 41, and is connected to the spiral feeding rod 40, so that the furnace body is kept sealed when the spiral feeding rod 40 rotates in the spiral feeding tube furnace system 100 of the present invention. In other embodiments, a plurality of rotary bearings may be disposed in the furnace tube 10 according to actual needs.
In the present embodiment, the first end 101 of the furnace tube 10 is communicated with the gas inlet device 70, the gas inlet device 70 has a first vent 71, a second vent 72 and a third vent 73, wherein the first vent 71 is configured as a vacuum pumping port and is connected to a vacuum pump (not shown) to vacuum the reaction chamber, the first vent 71 is provided with a vent valve 711 for controlling the opening or closing of the first vent 71; the second vent 72 is connected to a protective gas supply (not shown) for introducing a protective gas (e.g., argon) into the reaction chamber, and the second vent 72 is provided with a vent valve 721 for controlling the opening or closing of the second vent 72; the third vent 73 is indirectly communicated with the first end 101 of the furnace tube 10, and a pressure gauge is further disposed at an end close to the third vent 73 for monitoring the pressure inside the furnace tube 10 (reaction vessel) in real time.
The first heating system 51 surrounds the first heating zone furnace tube 12, and implements a heating function to provide a reaction temperature for the reaction chamber. The second heating system 52 surrounds the second heating zone furnace tube 13 to perform a heating function to provide a desired temperature to the product collection chamber. It is to be understood that in some embodiments, the first heating system 51 and the second heating system 52 of the present invention may be the same heating system, providing the same heating temperature to the first heating zone furnace tube 12 and the second heating zone furnace tube 13.
The product collecting device 60 is connected to the product collecting chamber (i.e. the second heating zone furnace tube) for collecting the powder product pushed to the product collecting chamber by the spiral feeding rod 40 (in the utility model, the reaction product powder is also the target product two-dimensional material, and of course, the reaction product powder can be other powder products according to different reactions). In this embodiment, the product collecting device 60 includes two storage tanks 61, 62, the two storage tanks 61, 62 are respectively communicated with the product outlet of the second heating zone furnace tube 13, and a first discharge flapper valve 63 and a second discharge flapper valve 64 are respectively disposed on the communicated connecting pipes; a connecting port 65 and a connecting port 66 are respectively arranged on the connecting pipes which are communicated with each other and are used for connecting a vacuum pump or a protective gas supply device so as to realize the function of vacuumizing or introducing protective gas into the material storage tanks 61 and 62, thereby avoiding the oxidation of product powder collected in the material storage tanks 61 and 62; the connection port 65 and the connection port 66 are further provided with a vent valve 651 and a vent valve 661 for controlling opening and closing of the connection port 65 and the connection port 66, respectively. In some embodiments, the product powder has oxidation resistance or stable properties in air, and the treatment of vacuumizing or introducing inert gas is not needed.
In another embodiment, the product collection device 60 can also be provided with a plurality of storage tanks (. Gtoreq.3) connected to the product collection chamber (i.e., the second heating zone furnace tube). The storage tanks are arranged more than two, so that the storage tanks can be used alternately, and continuous production is realized; for example, in the present embodiment, the first discharge flapper valve 63 is opened first, the second discharge flapper valve 64 is closed, the storage tank 61 is started, after the storage tank 61 is fully collected, the first discharge flapper valve 63 is closed, the second discharge flapper valve 64 is opened, the storage tank 62 is started, the classification is performed in sequence, and the storage tanks are pushed and used alternately, so as to realize continuous collection of the product powder. Of course, in another embodiment, such as a small batch production, the product collection device 60 may also be provided with a storage tank.
Example two
Referring to fig. 2, a second embodiment of the present invention provides another spiral feeding tube furnace system 200 for preparing two-dimensional materials, which is similar to the spiral feeding tube furnace system 100 of the first embodiment, except that in this embodiment, the furnace tube 10 is formed by flange-connecting each part of the tube members, except for the first connecting furnace tube 11, the first heating zone furnace tube 12 and the second heating zone furnace tube 13, the second connecting furnace tube 14 is connected to the second heating zone furnace tube 13 through the adapter flange 85, and is communicated with the gas outlet 103 through the sealing flange 84, and the spiral feeding rod 40 penetrates through the furnace tube 10. The interior of the second connecting furnace tube 14 is defined as a byproduct collecting chamber. The second connecting furnace tube 14 is also preferably made of a metal material (e.g., stainless steel) that is easy to machine and mold.
The spiral feeding tube furnace system 200 of the present embodiment further includes a byproduct collecting device 90, which is communicated with the byproduct collecting cavity (i.e., the second connecting furnace tube 14), similar to the product collecting device 60, the byproduct collecting device 90 includes a byproduct storage tank 91, the byproduct storage tank 91 is communicated with the second connecting furnace tube 14, the communicated connecting tubes are respectively provided with a third discharging baffle valve 92, and the communicated connecting tubes are further provided with a connecting port 93, so as to realize the function of vacuumizing or introducing protective gas into the byproduct storage tank 91, thereby avoiding the byproduct powder collected in the byproduct storage tank 91 from being oxidized; a vent valve 931 is further provided to the connection port 93 to control opening and closing of the connection port 93. In some embodiments, the byproduct powder itself is oxidation resistant or stable in air, and may not be treated with vacuum or protective gas.
In other embodiments, the byproduct collecting device 90 may also include a plurality of storage tanks (2 or more) for continuous collection of byproduct powder, so as to achieve alternate use.
The second connecting furnace tube 14 and the byproduct collecting device 90 added in this embodiment are used for collecting powder materials generated after gas phase condensation in the furnace tube 10. In actual production, reaction gas is introduced into the furnace tube 10 through the gas inlet device 70, and passes through the reaction chamber (first heating zone furnace tube 12), so that the reaction gas and reaction raw materials (powder materials) undergo gas-solid reaction to produce gas-phase byproducts; that is, after passing through the first heating zone furnace 12, the gas phase composition of the gas in the furnace 10 includes excess reactant gas and gas phase by-products. Because the second heating system 52 is provided to provide heat to a desired temperature, the gases in the second heating zone furnace tube 13 are still maintained in a gas phase, and continue to enter the second connecting furnace tube 14 (byproduct collecting cavity), in the second connecting furnace tube 14, part or all of the gases are condensed into byproduct powder, and the byproduct powder enters the byproduct collecting device 90 through the rotation propulsion of the spiral feeding rod 40, and meanwhile, the collection of the byproduct powder generated after condensation in the reaction system is realized.
In other embodiments, in order to rapidly condense the gas in the second connecting furnace tube 14, a cooling device, such as a circulating water cooling device, may be disposed outside the second connecting furnace tube 14 to achieve rapid condensation of the by-products into powder for collection.
EXAMPLE III
Referring to fig. 3, a third embodiment of the present invention provides another spiral-feed tube furnace system 300 for preparing two-dimensional materials, similar to the spiral-feed tube furnace system 100 of the first embodiment, except that a byproduct collecting device 90 is connected to the gas outlet 103 in this embodiment, for cooling and condensing the gas flowing out from the gas outlet 103 of the furnace tube 10 into powder for collection, wherein the gas phase component of the gas includes excess reaction gas and gas phase byproducts. In this embodiment, the byproduct collecting apparatus 90 includes a storage container 96 having a gas exhaust valve 961 for exhausting uncondensed gas, and a cooling apparatus 97, more specifically, a circulating water cooling apparatus, disposed outside the storage container 96. In actual production, vent valve 94 is opened, vent valve 95 is closed, and the gas discharged from gas outlet 103 can be collected in byproduct collecting device 90.
Example four
The fourth embodiment of the present invention provides a method for using the spiral feed tube furnace system 100 for preparing two-dimensional material, which comprises the following steps:
s11, placing a certain amount of powder materials in a feeder 20, closing a baffle valve 23, opening a gas valve 221, vacuumizing a connecting pipe 22, and then introducing protective gas to normal pressure;
s12, opening the vent valve 711, vacuumizing the furnace tube 10 from the first vent hole 71, closing the vent valve 711, opening the vent valve 721, introducing protective gas into the furnace tube 10 from the second vent hole 72, and stopping introducing the protective gas after the interior of the furnace tube is returned to the normal pressure state;
s13, introducing reaction gas into the furnace tube 10 from the second vent 72 to fill the interior of the furnace tube 10 with the reaction gas, then opening the first heating system 51 to heat the reaction chamber of the furnace tube 12 of the first heating zone to the reaction temperature required for preparing the two-dimensional material, and preserving the heat;
s14, opening the feeder 20, the baffle valve 23 and the rotating motor 30, and driving the spiral feeding rod 40 by using the rotating motor 30 to send the powder material in the feeder 20 into the reaction chamber of the furnace tube 12 of the first heating zone to carry out gas-phase reaction to prepare the two-dimensional material;
s15, opening the second heating system 52, heating the product collecting chamber of the furnace tube 13 of the second heating zone to a certain temperature, and preserving the heat; and
s16, opening a first discharging baffle valve 63, and collecting the two-dimensional reaction product material in a storage tank 61; when the storage tank 61 is full, the first discharge flapper valve 63 is closed, the second discharge flapper valve 64 is opened, and the two-dimensional reaction product material is collected in another storage tank 62, which can be used alternately during continuous production.
EXAMPLE five
The fifth embodiment of the present invention provides another method for using a spiral-feed tube furnace system 100 for preparing two-dimensional materials, which comprises the following steps:
s21, placing a certain amount of mixed materials in the feeder 20, wherein the mixed materials comprise powder materials and a reactant, and the reactant powder can be sublimated into a gaseous state by heating in the furnace tube 10 to realize the reaction of the gaseous reactant and the powder materials; closing the baffle valve 23, opening the gas valve 221, vacuumizing the connecting pipe 22, and introducing protective gas to normal pressure;
s22, opening the vent valve 711, vacuumizing the furnace tube 10 from the first vent hole 71, closing the vent valve 711, opening the vent valve 721, introducing protective gas into the furnace tube 10 from the second vent hole 72, and stopping introducing the protective gas after the interior of the furnace tube is returned to the normal pressure state;
s23, opening the first heating system 51, heating the reaction chamber of the first heating zone furnace tube 12 to the reaction temperature required for preparing the two-dimensional material, and preserving the heat;
s24, opening the baffle valve 23 and the rotary motor 30 of the feeder 20, driving the spiral feeding rod 40 by using the rotary motor 30 to feed the mixed materials in the feeder 20 into the reaction chamber of the furnace tube 10, heating and sublimating (vaporizing) the reactants in the mixed materials in the reaction chamber, and carrying out gas phase reaction to prepare the two-dimensional material;
s25, opening the second heating system 52, heating the product collecting chamber of the furnace tube 13 of the second heating zone to a certain temperature, and preserving the heat; and
s26, opening a first discharging baffle valve 63, and collecting the two-dimensional reaction product material in a storage tank 61; when the storage tank 61 is full, the first discharge flapper valve 63 is closed, the second discharge flapper valve 64 is opened, and the two-dimensional reaction product material is collected in another storage tank 62, which can be used alternately during continuous production.
In step S11 or S21, the powder material is a raw material for preparing a two-dimensional material, and is related to the kind of the two-dimensional material. In a specific embodiment, the powder material is a MAX phase material and/or an MXene material, a MAX phase material, such as Ti 3 AlC 2 MXene materials such as Ti 3 C 2 T x Of course, alternative types of MAX phase or MXene materials may be substituted.
The furnace tube 10 and the feeder 20 are opened, vacuumized, and then filled with protective gas, so as to prevent air from entering the furnace tube 10 and affecting the reaction.
In step S12, in some embodiments, a mixed gas of a reactive gas and a protective gas is introduced from the ventilation valve 721; the protective gas is inert gas such as argon and the like; the reaction gas is a gas capable of chemically reacting with the powder material, and comprises halogen hydride (such as HCl, HBr, HI), iodine vapor, and sulfur-group hydride (such as H) 2 S、H 2 Se、H 2 Te), ammonia gasPhosphine, and the like. In other embodiments, the protective gas and the reactive gas may be introduced sequentially, such as introducing the protective gas first and then introducing the reactive gas. In one embodiment, a mixture of hydrogen chloride (HCl) and argon is introduced.
In step S21, in some embodiments, the powder material in the mixed material is a MAX phase material and/or an MXene material, and the reactant is elemental chalcogen powder, such as sulfur powder, selenium powder, and tellurium powder, or solid powder decomposed to generate chalcogen hydride, such as ammonium sulfide, or a low boiling point (boiling point < 1000 ℃) metal halide salt.
In step S13 or S23, the reaction temperature is related to the type of the two-dimensional material or the type of the powder material, and generally ranges from 300 ℃ to 1500 ℃. In one embodiment, the powder material is Ti 3 AlC 2 The reaction temperature was 700 ℃.
In step S14 or S24, the speed of the spiral feeding rod 40 is 0.01cm/min to 100cm/min, which is related to the reaction speed of the reaction gas and the powder material, and the residence time of the reaction raw material powder material in the furnace tube 12 of the first heating zone, i.e., the reaction time, can be controlled by the speed of the spiral feeding rod 40. Preferably, the speed of the screw feed bar 40 is 1cm/min, 10cm/min, 20cm/min, 40cm/min, 60cm/min, 80cm/min, 100cm/min. In one embodiment, the speed of the spiral feeding rod 40 is 10cm/min, the length of the first heating zone furnace tube 12 is 3m, and the residence time (reaction time) of the reaction raw material powder material in the first heating zone furnace tube 12 is controlled to about 30min; the length of the second heating zone furnace tube is 1m, and the residence time in the second heating zone furnace tube 13 is about 10min.
In step S15 or S25, the temperature of the product collection chamber of the second heating zone furnace tube 13 is also related to the type of the two-dimensional material or the type of the powder material, and the temperature of the product collection chamber should be equal to or higher than the boiling point temperature of the byproduct and lower than the melting point of the two-dimensional material, so that the byproduct can be prevented from being condensed on the tube wall at one end of the furnace tube 10, and the structure of the target product two-dimensional material can be prevented from being damaged. In one embodiment, the powder material isTi 3 AlC 2 The reaction gas is HCl or Ti 3 AlC 2 Reacting with HCl to obtain MXene material with accordion shape and byproduct AlCl 3 (boiling point 178 ℃), the temperature of the product collection chamber of the second heating zone furnace tube 13 is therefore set at > 178 ℃, preferably in the range 200 ℃ to 400 ℃.
EXAMPLE six
The sixth embodiment of the present invention provides another method for using the spiral feeding tube furnace system 200 for preparing two-dimensional materials, which is similar to the fourth and fifth embodiments, except that the gas in the furnace tube 10 is condensed into powder by-product and/or unnecessary reaction gas when passing through the second connecting furnace tube 14, and the by-product powder enters the by-product storage tank 91 of the by-product collecting device 90 through the rotation of the spiral feeding rod 40.
EXAMPLE seven
The seventh embodiment of the present invention provides another method for using the spiral-feeding tube furnace system 300 to prepare two-dimensional materials, which is similar to the fourth and fifth embodiments, except that the gas in the furnace tube 10 enters the byproduct collecting device 90 after passing through the gas outlet 103, and the gaseous byproduct and/or the excessive reaction gas are condensed into powder byproduct powder and stored in the storage container 96.
Example eight
The eighth embodiment of the present invention provides a method for using a spiral feeding tube furnace system to continuously produce and prepare two-dimensional materials, which is described by taking the spiral feeding tube furnace system 100 as an example, wherein the feeder 20 is an automatic feeder, and can continuously convey the powder material in the storage container 21 to the furnace tube 10 at a predetermined speed, and more specifically, the powder material enters the cavity of the first connecting furnace tube 11 through the connecting pipeline.
Before the continuous production preparation, the furnace tube 10 is vacuumized and then filled with protective gas (argon), and the first heating system 51 and the second heating system 52 are started to raise the furnace temperature to a predetermined temperature; starting the rotating motor 30 to drive the spiral feeding rod 40 to rotate; opening the first discharge flapper valve 63, closing the second discharge flapper valve 64, and opening the third discharge flapper valve 92;
the feeder 20 is started again, the powder material enters the furnace tube 10, enters the reaction chamber in the first heating zone furnace tube 12 along with the rotation of the spiral feeding rod 40 to perform gas-solid reaction, and enters the product collection chamber in the second heating zone furnace tube 13 under the driving of the rotation of the spiral feeding rod 40, and then enters the material storage tank 61 of the product collection device 60 through the product collection port; when the storage tank 61 is nearly full, the first discharge baffle valve 63 is closed, and the second discharge baffle valve 64 is opened, so that the reaction product powder enters the storage tank 62, and the two storage tanks are alternately used, thereby realizing continuous production and preparation.
Detailed description of the preferred embodiment 1
The MAX phase material is Ti 3 AlC 2 The use of the spiral-feed tube furnace system 200 for producing two-dimensional materials in the present invention, or MXene Ti produced using the spiral-feed tube furnace system 200, is illustrated by way of example of a commercial HCl liquefied gas as the halogen hydride gas 3 C 2 Cl x A method of two-dimensional material comprising the steps of:
(1) 2kg of powdered MAX phase material Ti was placed in the feeder 20 3 AlC 2 Closing the baffle valve 23, opening the gas valve 221, and closing the feeder 20 after vacuumizing;
(2) Opening the vent valve 711, and performing vacuum-pumping treatment on the furnace tube 10;
(3) Closing the vent valve 711, opening the vent valve 721, and introducing the mixed gas of argon and HCl from the second vent 72 to fill the interior of the furnace tube 10 with the mixed gas; preferably, the volume fraction of HCl in the mixed gas is between 5% and 50%, and in one embodiment, the mixed gas with 10% of HCl is selected;
(4) Opening the first heating system 51 to heat the reaction chamber of the first heating zone furnace tube 12 to 700 ℃, and performing heat preservation treatment;
(5) The feeder 20 and the rotary motor 30 were opened, the speed of the screw feed rod 40 was adjusted to 1cm/min, and the powder material in the feeder 20 was fed into the reaction chamber of the first heating zone furnace tube 12 by the screw feed rod 40 to be subjected to gas phaseReacting to prepare two-dimensional material, specifically HCl gas and MAX phase material Ti 3 AlC 2 Etching reaction occurs, HCl etches Ti 3 AlC 2 Al element in the MXene to generate MXene material Ti 3 C 2 Cl x And AlCl as a by-product 3 (boiling point 178 ℃ C.);
(6) The second heating system 52 is turned on to heat the product collecting chamber of the second heating zone furnace tube 13 to 400 ℃, and the heat preservation treatment is carried out, at the temperature, the by-product AlCl is generated 3 Is in a gaseous state;
(7) Opening a first discharge baffle valve 63, and continuously collecting reaction product powder (two-dimensional material) in a storage tank 61;
(8) The third discharge flapper valve 92 is opened to remove the by-product powder (AlCl) 3 ) Continuously collected in the byproduct storage tank 91, in the embodiment of the spiral feed tube furnace system 200, the byproduct AlCl 3 Cooled in the byproduct collection chamber of the second connecting furnace tube 14 and condensed into solid AlCl 3 Powder, the solid AlCl is fed by rotation of the screw-feeding rod 40 3 Collecting the powder in a byproduct storage tank 91 to obtain high-purity AlCl 3 Chemicals, excess gases (including unreacted HCl, argon, etc.) are vented through vent 103.
In the specific embodiment 1, after the reactants in the feeder 20 are fed and all the precursors are reacted, the temperature of the reaction apparatus is reduced, and the target product MXene Ti in the storage tank 61 is taken out 3 C 2 Cl x . FIG. 4 is a 10 kilogram grade MXene Ti produced using a spiral feed tube furnace system 200 3 C 2 Cl x An optical photograph of (a). For MAX phase materials Ti 3 AlC 2 And MXene Ti as a target product 3 C 2 Cl x Scanning Electron Microscope (SEM) tests were performed, respectively, and the results are shown in fig. 5. In FIG. 5, a is a MAX phase material Ti 3 AlC 2 SEM photograph of (5), B in FIG. 5 is MXene Ti 3 C 2 SEM photograph of Clx. As can be seen by comparing a and b in FIG. 5, ti 3 AlC 2 The appearance of the compound is a three-dimensional blocky structure, and the target product MXene Ti 3 C 2 Cl x A pronounced accordion-like layered structure appears.
For MAX phase material Ti 3 AlC 2 And MXene Ti as a target product 3 C 2 Cl x The result of X-ray diffraction (XRD) analysis was as shown in FIG. 6, and Ti as a raw material was used 3 AlC 2 The (002) peak in (b) appears at the 9.5 ℃ position, and MXene Ti, the target product after reaction with hydrogen chloride (HCl) 3 C 2 Cl x The (002) peak in (III) was shifted to 8.0 ℃ at a low angle, indicating that the HCl gas completely etched Ti in the gas phase etching reaction 3 AlC 2 Al element in the alloy to form Ti with accordion-like structure 3 C 2 Cl x MXene, resulting in an enlargement of the interlayer spacing, which is comparable to Ti 3 C 2 T x The results of the scanning electron micrographs are consistent. XRD test of the target product can also show that the product does not contain characteristic peak of MAX phase material of raw material, which indicates the high purity of the obtained product.
Comparative example 1
MXene Ti prepared by using common tube furnace 3 C 2 Cl x A method of two-dimensional material comprising the steps of:
(1) 2kg of powdered Ti was placed inside a general tube furnace 3 AlC 2 ；
(2) Continuously introducing HCl gas into the tubular furnace to fill HCl gas into a reaction cavity in the tubular furnace;
(3) And (3) heating the tubular furnace to 700 ℃ for gas phase reaction to obtain the target product.
The material obtained in comparative example 1 was further subjected to XRD characterization, and as shown in FIG. 7, the product obtained in comparative example 1 showed simultaneous appearance of Ti corresponding to the 9.5 ° and 8.0 ° positions 3 AlC 2 And Ti 3 C 2 Cl x MXene (002) characteristic diffraction peak, and Ti is simultaneously present in the product 3 AlC 2 And Ti 3 C 2 Cl x It has been shown that it is difficult to achieve a large amount of complete conversion of MAX phase to MXene in a conventional tube furnace.
Specific example 2
This example provides for the preparation of MXene Ti 3 C 2 I x Method for using a spiral-feed tube furnace system 200 for two-dimensional materials, or for preparing MXene Ti using said spiral-feed tube furnace system 300 3 C 2 I x A method of two-dimensional material comprising the steps of:
(1) 2kg of powdered MAX phase material Ti was placed in the feeder 20 3 AlC 2 Mixed material (Ti) of solid iodine simple substance powder 3 AlC 2 And the iodine simple substance powder in a mass ratio of 1:10 Open the gas valve 221, and close the feeder 20 after evacuation;
(2) Opening the vent valve 711, performing vacuum pumping treatment on the furnace tube 10, closing the vent valve 711, opening the vent valve 721, and introducing argon gas from the second vent 72 until the furnace tube 10 returns to normal pressure;
(3) Opening the first heating system 51, heating the reaction chamber of the first heating zone furnace tube 12 to 700 ℃, and performing heat preservation treatment;
(4) Opening the feeder 20 and the spiral feeding rod 40, adjusting the speed of the spiral feeding rod 40 to 1cm/min, feeding the mixed material in the feeder 20 into the reaction chamber of the first heating zone furnace tube 12 by using the spiral feeding rod 40, and performing a gas phase reaction to prepare the two-dimensional material, specifically, subliming the iodine elemental powder into iodine vapor and MAX phase material Ti 3 AlC 2 Etching reaction occurs, iodine vapor etches Ti 3 AlC 2 Al element in the MXene to generate MXene material Ti 3 C 2 I x And byproduct AlI 3 (boiling point 382 ℃ C.);
(5) The second heating system 52 is turned on to raise the temperature of the product collection chamber of the second heating zone furnace tube 13 to 600 ℃, and the heat preservation treatment is carried out, at which temperature the byproduct AlI is 3 Is in a gaseous state;
(6) Opening the first discharge flapper valve 63 and/or the second discharge flapper valve 64 to continuously collect the reaction product two-dimensional material in the storage tank 61 and/or the storage tank 62;
(7) The third discharge flapper valve 92 is opened and the reaction intermediate (byproduct AlI) is removed 3 ) Continuously collecting the gas in the byproduct storage tank 91, when the gas in the furnace tube 10 passes through the second connecting furnace tube 14, the furnace temperature is reduced, and byproduct AlI is generated 3 Condensed into solid powder, pushed into a byproduct storage tank 91 along with the rotation of the spiral feeding rod 40 and collected to obtain high-purity AlI 3 A chemical.
In some embodiments, the evacuation process in this embodiment may be replaced by introducing a protective gas to remove air from the furnace 10 and/or the feeder 20.
In some embodiments, the reactant in this embodiment may be replaced by other chemical capable of sublimating or vaporizing by heating, and for the MAX phase material powder, the reactant having etching effect may be ammonium halide (such as NH) 4 Cl、NH 4 I, etc.), halogenated metal salts (e.g., znCl) 2 、CuCl 2 Etc.), adjusting the temperatures of the first and second heating systems according to the characteristics of the different reactants, thereby realizing the preparation of the two-dimensional material.
Specific example 3
The process of this example is similar to that of example 2, except that Ti is used as the mixing material 3 AlC 2 And ZnCl 2 Elemental powder, in step 3, the first heating system 51 is turned on to raise the temperature of the reaction chamber of the furnace tube 12 of the first heating zone to 1000 ℃, and heat preservation treatment is performed; in step 5, the second heating system 52 is turned on to raise the temperature of the product collection chamber of the second heating zone furnace tube 13 to 800 ℃, and the heat preservation treatment is performed, at which temperature the by-product AlCl is generated 3 And excess ZnCl 2 Is in a gaseous state.
Specific example 4
This example provides a method for using the spiral-feeding tube furnace system 100 for preparing a transition metal chalcogenide two-dimensional material, or a method for preparing a transition metal chalcogenide two-dimensional material using the spiral-feeding tube furnace system 100, to prepare MoS 2 By way of example, the method comprises the following steps:
(1) 2kg of a powdery MAX phase material Mo was placed in a feeder 20 2 GeC；
(2) Argon and H are introduced from the vent valve 721 2 S, the mixed gas is filled in the furnace tube 10; preferablyH in the mixed gas 2 The volume fraction of S is between 5% and 50%, and in one embodiment, H is introduced 2 Mixed gas with the volume fraction of S being 10 percent;
(3) Opening the first heating system 51, heating the reaction chamber of the first heating zone furnace tube 12 to 800 ℃, and performing heat preservation treatment;
(4) Opening the feeder 20 and the spiral feeding rod 40, adjusting the speed of the spiral feeding rod 40 to 0.2cm/min, feeding the powder material in the feeder 20 into the reaction chamber of the first heating zone furnace tube 12 by using the spiral feeding rod 40, and performing a gas phase reaction to prepare the two-dimensional material, specifically, H 2 S gas and MAX phase material Mo 2 GeC has topology conversion reaction, and Mo is replaced by S element 2 Ge element and C element in GeC to generate MoS 2 And by-product germanium hydride (GeH) 4 Gaseous at room temperature);
(5) Opening the first discharge damper 63 and/or the second discharge damper 64 to continuously collect the reaction product two-dimensional material in the storage tank 61 and/or the storage tank 62;
(6) The reaction intermediate (by-product GeH) 4 ) And is discharged through gas outlet 103.
In this embodiment, the second heating system 52 is not required to be used, and it can be understood that the temperature set by the second heating system 52 is normal temperature.
Specific example 5
This example provides a method for using the spiral-feeding tube furnace system 300 for preparing a transition metal chalcogenide two-dimensional material, or a method for preparing a transition metal chalcogenide two-dimensional material using the spiral-feeding tube furnace system 300, to prepare MoS 2 By way of example, the method comprises the following steps:
(1) 2kg of a powdery MXene material Mo was placed in a feeder 20 2 Mixture of C and elemental sulphur powder, mo 2 The molar ratio of C to elemental sulfur powder is 1: (1-1.5);
(2) Introducing argon gas from the vent valve 721 to fill the furnace tube 10 with argon gas;
(3) Opening the first heating system 51, heating the reaction chamber of the first heating zone furnace tube 12 to 800 ℃, and performing heat preservation treatment;
(4) Opening the feeder 20 and the spiral feeding rod 40, adjusting the speed of the spiral feeding rod 40 to 0.5cm/min, feeding the mixed material in the feeder 20 into the reaction chamber of the first heating zone furnace tube 12 by using the spiral feeding rod 40, and performing a gas phase reaction to prepare the two-dimensional material, specifically, heating and subliming elemental sulfur powder into a gas state, and mixing the gas state with MXene material Mo 2 C undergoes a topology transformation reaction, and the element S replaces the element C to generate MoS 2 ；
(5) Opening the second heating system 52, heating the product collecting chamber of the second heating zone furnace tube 13 to 200 ℃, and carrying out heat preservation treatment, wherein at the temperature, the elemental sulfur is in a gaseous state;
(6) Opening the first discharge damper 63 and/or the second discharge damper 64 to continuously collect the reaction product two-dimensional material in the storage tank 61 and/or the storage tank 62;
(7) The third discharge damper 92 is opened, the gas in the furnace tube 10 enters the storage container 96 through the gas outlet 103, and because the cooling device 97 is arranged outside the storage container 96, the gaseous sulfur is condensed into solid elemental sulfur powder in the storage container 96 and can be recycled, and the redundant gas is discharged through the exhaust valve 961.
In this embodiment, the sulfur powder may also be replaced with other elemental powders of chalcogen, such as selenium powder, tellurium powder, and the like, to obtain a two-dimensional transition metal chalcogenide.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application, to thereby enable others skilled in the art to make and utilize various exemplary embodiments of the invention and various alternatives and modifications. It is intended that the scope of the invention be defined by the claims and their equivalents.

Claims (10)

1. A spiral feeding tube furnace system for preparing two-dimensional materials is characterized by comprising a furnace tube, a feeder, a rotary motor, a spiral feeding rod, a first heating system, a second heating system and a product collecting device;
the feeder is connected with the furnace tube and is used for feeding powder materials into the furnace tube;
the furnace tube comprises a reaction chamber and a product collection chamber;
the rotary motor is connected with the spiral feeding rod, and the powder material is driven to move in the furnace tube through the rotation of the spiral feeding rod and sequentially passes through the reaction chamber and the product collecting chamber;
the first heating system surrounds the reaction chamber and the second heating system surrounds the product collection chamber;
the product collecting device is connected with the product collecting chamber and is used for collecting the powder pushed by the spiral feeding rod.
2. A spiral feed tube furnace system for producing two dimensional materials as recited in claim 1 wherein said furnace tube comprises: connecting the furnace tube, the first heating zone furnace tube and the second heating zone furnace tube; the connecting furnace tube is connected with the feeder, the first heating system surrounds the first heating zone furnace tube, and the interior of the first heating zone furnace tube is defined as the reaction chamber; the second heating system surrounds the second heating zone furnace tube, the second heating zone furnace tube interior being defined as the product collection chamber.
3. The spiral-feed tube furnace system for preparing two-dimensional materials as claimed in claim 1 or 2, wherein a plurality of product outlets are arranged in the product collection chamber and are respectively connected with the storage tank of the product collection device.
4. The spiral feed tube furnace system for producing two-dimensional materials of claim 3, wherein the connecting pipe of each of said product discharge ports and said storage tank is provided with a discharge flapper valve;
and/or a vent is arranged on a connecting pipe fitting of each product discharge port and the storage tank and is used for vacuumizing and/or introducing protective gas into the storage tank.
5. The spiral feed tube furnace system for producing two-dimensional materials of claim 1 wherein said furnace tube has opposite first and second ends, said first end being connected to a gas inlet means and said second end being connected to a gas outlet; the air inlet device is provided with a first air inlet and a second air inlet, the first air inlet is used for being connected with the vacuumizing device, and the second air inlet is used for being connected with the protective gas supply device.
6. The spiral feed tube furnace system for producing two-dimensional materials as claimed in claim 1, wherein a rotary bearing is disposed in the furnace tube for fixedly supporting the spiral feed rod to rotate the spiral feed rod.
7. The spiral-feed tube furnace system for producing two-dimensional materials of claim 1, wherein the spiral-feed tube furnace system comprises a sealed magnetic fluid flange and/or a plurality of adapter flanges.
8. The spiral feeding tube furnace system for preparing the two-dimensional material as claimed in claim 7, wherein the rotary motor and the spiral feeding rod form a spiral feeding device, and the sealing magnetic fluid is used for flange connection of the furnace tube and the spiral feeding device to realize the sealing effect under the rotation condition of the spiral feeding rod;
and/or the adapter flange is used for assembling and connecting furnace tube components and has the functions of connection and sealing.
9. The spiral feeding tube furnace system for preparing two-dimensional materials according to claim 1, wherein the feeder continuously feeds reaction raw material powder into the furnace tube within a predetermined period of time to realize continuous preparation.
10. The spiral-fed tube furnace system for producing two-dimensional materials of claim 1, wherein said first heating system and said second heating system are the same heating device.
CN202222984715.8U 2022-11-09 2022-11-09 Spiral feeding tube furnace system for preparing two-dimensional material Active CN218673102U (en)

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