CN109809374B - Push boat type semi-continuous boron nitride nanotube preparation furnace and use method thereof - Google Patents
Push boat type semi-continuous boron nitride nanotube preparation furnace and use method thereof Download PDFInfo
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Abstract
The invention relates to a push boat type semicontinuous boron nitride nanotube preparation furnace and a using method thereof. The device comprises an electric control temperature heating device A, a furnace body B, a furnace head C and a furnace tail D, wherein the electric control temperature heating device A is used for adjusting and controlling the temperature of the furnace body B, a hearth in the furnace body B is communicated with the furnace head C and the furnace tail D on two sides through a furnace tube, and a circulating water support for cooling is arranged on the outer surface of the furnace tube. The raw materials react with ammonia gas in the furnace body B hearth, then are transferred into the furnace tube between the furnace body B and the furnace tail D for cooling, meanwhile, the next batch of raw materials are conveyed into the furnace hearth for reaction, and the cooled product is taken out from the furnace tail D, so that continuous production is realized. The device has the advantages of convenient operation, rich and various product structures, high equipment safety, good stability, capability of continuously synthesizing BNNTs with different structures on a large scale, and the like, and is particularly suitable for industrial production and application.
Description
Technical Field
The invention relates to the technical field of synthesis of machinery and inorganic non-metallic materials, in particular to a push boat type semi-continuous boron nitride nanotube preparation furnace and a using method thereof.
Background
The synthesis method of Boron Nitride (BN) plays an extremely important role in the research of boron nitride materials. Develops a method for industrially synthesizing high-purity boron nitride on a large scale, and can provide solid foundation and guarantee for theoretical research and practical application of boron nitride.
Boron Nitride Nanotubes (BNNTs) are important materials among many boron nitride materials, and have excellent mechanical, thermal, and electromagnetic properties. The existing BNNTs preparation method mainly comprises an arc discharge method, a laser ablation method, a vapor deposition method (CVD), a high-temperature synthesis method and the like. The arc discharge method directly uses reaction raw materials as electrodes, and then obtains target materials through arc discharge, and BNNTs is prepared by the method for the first time. However, the method has high energy consumption and is not suitable for mass production. The laser ablation method utilizes laser to bombard the massive reactants in the atmosphere of high-pressure inert gas to obtain the required product, and has the defects of high energy consumption, low yield and unsuitability for industrial popularization and industrialization. Chemical Vapor Deposition (CVD) basic principle: the gas reactant is contacted with the solid reactant in the active atmosphere to carry out chemical reaction, and finally, a stable solid product is obtained. The method has the following three necessary conditions for success: (1) the reactants have sufficient vapor pressure at the deposition temperature and can be introduced into the reaction chamber at an appropriate rate; (2) the reactants, except for the formation of solid film materials, must be volatile; (3) the deposited film and the base material must have a sufficiently low vapor pressure. Thus, the CVD method has high equipment requirements, great limitations, and is generally more used for preparing coating materials.
The high-temperature synthesis method is the most common method, and comprises the steps of fully mixing proportioned raw materials to uniformly disperse the raw materials, carrying out physical and chemical reaction in a high-temperature environment to generate a crude product, and finally carrying out impurity removal, drying and other processes to obtain a target product. The method has the advantages of simple operation, relatively low requirement on equipment and the like. The high-temperature synthesis equipment with stable performance, safety and reliability is the basic guarantee for the full reaction of the raw materials at high temperature. Chinese patent CN201359434Y discloses a push boat type two-tube reducing furnace, and is used for reducing metal powder, but on one hand, the device has more complex structure, more temperature control areas and small temperature difference, and has no great significance for the synthesis of BNNTs; on the other hand, the device is not provided with a gas circulation system, and the effective utilization rate of the reducing gas is not high. Chinese patent CN104555990A discloses a carbonization and graphitization continuous high temperature furnace and its use method, and is respectively used for synthesis of graphite materials. However, the equipment cannot create the atmosphere required by the reaction, and waste gas generated by the reaction cannot be effectively treated, so that the environmental protection problem exists; in addition, the equipment has different temperature reaction zones, so that more heating equipment is required, materials need to be pushed in different reaction zones, and the operation is inconvenient.
Disclosure of Invention
The invention provides a push boat type semicontinuous boron nitride nanotube preparation furnace, which belongs to a semicontinuous preparation device, reduces unnecessary cooling time from high temperature to low temperature of the device, greatly reduces energy consumption, prolongs the service life, and is particularly suitable for rapidly and massively synthesizing BNNTs of various precursors of different types at different temperatures (the maximum temperature can reach 1600 ℃). In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a push boat type semi-continuous boron nitride nanotube preparation furnace comprises an electric control heating device A, a furnace body B, a furnace head C, a furnace tail D and a push rod. The electric control heating device A is fixed on the furnace body B and is used for heating the furnace body B under a controlled condition; a furnace end exhaust pipe 1 is arranged on the furnace end C, and a furnace tail air inlet pipe 2 is arranged on the furnace tail D; the furnace head C and the furnace tail D are communicated with a hearth 8 in the furnace body B through a furnace tube 14 to form a complete gas inlet and outlet channel. The push rod can enter the hearth 8 of the furnace head B through the furnace head C and the furnace tube 14, and pushes the product in the hearth 8 to the furnace tube between the furnace tail D and the furnace body B. This, on the one hand, makes room for the next batch to react and, on the other hand, transfers the product of the reaction to a cooling zone for cooling for tapping.
Further, the electric control heating device A comprises an electric control cabinet and a heating element (1800 type high-temperature silicon-molybdenum rod), and the electric control cabinet can control the heating element to heat and raise the temperature of the furnace body B according to a set program, so that the temperature in the hearth is stabilized at a set value. The electric control heating device A adopts PID intelligent program temperature control, integrates the integrated comprehensive control functions of temperature control and electric appliance control, and the main control circuit is a temperature control loop consisting of a bidirectional thyristor, a self-coupling transformer, a relay and an intelligent temperature control instrument. The intelligent temperature control instrument adopts digital display, the measurement precision is 0.3 grade, 30 sections of program temperature control can be realized, the temperature control precision can reach +/-1 ℃, the control mode adopts an over-phase contact method, and the instrument can be manually or automatically adjusted.
The furnace body B comprises a furnace shell 7, a hearth 8, a furnace lining 9 and a heat-insulating layer 10. The furnace body B is internally provided with a furnace lining 9 surrounding a hearth 8, and the furnace lining 9 is externally coated with a heat-insulating layer 10 and a furnace shell 7. The furnace shell 7 is formed by machining a 304 stainless steel plate, has enough strength and rigidity and attractive appearance, and adopts a double-layer air cooling structure as a whole. The hearth 8 is formed by processing 1700 type crystal fibers produced by Isularte in Shanghai; the furnace lining 9 is a composite furnace lining formed by filling 1600-type alumina hollow balls, and has the advantages of good heat insulation performance, rapid heat and rapid cooling resistance, no need of considering the influence of thermal stress, energy conservation, high strength, no deformation and the like; the heat-insulating layer 10 is built by 1500 type high-quality mullite light heat-insulating bricks. The furnace bottom adopts high-temperature mullite heat-insulating bricks to support the furnace tube, so that the furnace tube is prevented from heating deformation.
The furnace end C comprises a furnace end exhaust pipe 1, a furnace end furnace door 3, a furnace end sealing cover 5, a furnace end table 11 and a furnace end circulating water support 15-1. The furnace end exhaust pipe 1 is communicated with the furnace pipe 14 and is used for vacuumizing and discharging waste gas in the hearth; the furnace end circulating water support 15-1 is sleeved on the outer surface of the furnace tube 14, and one end of the furnace end circulating water support is fixed on the furnace end table 11, and the other end of the furnace end circulating water support is fixed on the furnace body B through a flange 16. The furnace end circulating water support can play the role of fixing and supporting equipment such as a furnace tube and preventing the equipment from moving on the one hand, and can cool the furnace tube and the like through cooling water on the other hand. The furnace end sealing cover 5 wraps the furnace end table 11, the furnace end circulating water support 15-1 and the like and seals the furnace end table and the furnace end circulating water support, the furnace end exhaust pipe 1 is arranged on the furnace end sealing cover 5, and the furnace end furnace door 3 is arranged at one end of the furnace pipe 14.
The furnace tail D is similar to the furnace head C in structure and comprises a furnace tail air inlet pipe 2, a furnace tail sealing cover 6, a furnace tail furnace door 4, a furnace tail table 12 and a furnace tail circulating water support 15-2. The furnace tail gas inlet pipe 2 is communicated with the furnace tube 14 and is used for conveying feed gas ammonia gas into the hearth; the furnace tail circulating water support 15-2 is sleeved on the outer surface of the furnace tube 14 to form a cooling area, one end of the furnace tail circulating water support 15-2 is fixed on the furnace tail table 12, and the other end is fixed on the furnace body B through a flange 16. The effect of the furnace tail circulating water support is similar to that of the furnace head circulating water support. The furnace tail sealing cover 6 wraps the furnace tail table 12, the furnace tail circulating water support 15-2 and the like and seals the furnace tail table and the furnace tail circulating water support, the furnace tail sealing cover 6 is provided with a furnace tail air inlet pipe 2, and the furnace tail furnace door 4 is arranged at the other end of the furnace pipe 14.
Further, a stainless steel pipe 13 and a stainless steel protective cover are arranged on the outer surfaces of the furnace tail circulating water support 15-1 and the furnace head circulating water support 15-2, adjusting bases 18 are arranged at the bottoms of the furnace head table 11 and the furnace tail table 12, and the furnace tail circulating water support 15-1 and the furnace head circulating water support 15-2 are connected with cooling water.
Further, a gas circulation device, such as a pipeline gas circulation machine (model number SMTD _ XHJ _ B100, manufactured by mitsungming fluid equipment limited, collocated with SMTD _ B _100 booster pump) is also provided between the furnace end exhaust pipe 1 and the furnace tail intake pipe 2.
The use method of the push boat type semi-continuous boron nitride nanotube preparation furnace comprises the following steps: (a) firstly, starting an electric control heating device A, and setting the temperature to heat a hearth 8 of a furnace body B; (b) then closing a furnace end furnace door 3 and a furnace tail furnace door 4, opening a furnace end exhaust pipe 1 and a furnace tail gas inlet pipe 2, vacuumizing a hearth 8 so as to exhaust air as far as possible, continuously conveying ammonia gas into the hearth 8 through the furnace tail gas inlet pipe 2, and then putting the ceramic boat fully covered with boron carbide powder into the hearth 8 for heat preservation reaction; (c) after the reaction is finished, opening a furnace end furnace door 3 of a furnace end C, moving the ceramic boat to a cooling area between a furnace body B and a furnace tail D by using a push rod for annealing, and simultaneously putting the other ceramic boat which is fully paved with boron carbide powder into a hearth 8 for reaction; (d) and (c) repeating the step (c), taking out the annealed ceramic boat from a furnace tail furnace door 4 of the furnace tail D, and carrying out aftertreatment on the obtained product to obtain the boron nitride nanotube.
Further, the flow rate of ammonia gas is 0.4-1.2L/min, and the heating rate of the hearth is 4-10 ℃/min.
Further, the ceramic boat fully paved with the boron carbide powder is heated to the temperature of 900-1400 ℃, and the reaction is carried out for 3-15h under the condition of heat preservation.
Further, the post-treatment comprises the processes of acid washing, water washing, filtering, drying and the like, and the specific process comprises the following steps: and (3) putting the product into 10-20 wt% HCl solution for soaking for 8-16h, then filtering and washing until the filtrate is neutral, and finally putting the filter cake in an environment of 60-90 ℃ for heat preservation for 8-16 h.
Compared with the prior art, the invention has the following beneficial effects: (1) the device is convenient to operate, reaction raw materials and operation process are easy to adjust, and the prepared product has rich and various structures and is particularly suitable for industrial production and application;
(2) the gas circulation device arranged between the furnace head and the furnace tail not only ensures the reaction gas (NH)3) The method is fully and effectively utilized, and is also beneficial to regulating and controlling the technological parameters of the annealing reaction and improving the yield;
(3) the device is simple to assemble, high in equipment safety and good in stability, not only can effectively improve the synthesis rate and the production capacity, but also has high thermotechnical control integration, and is beneficial to accurate control and adjustment of reaction temperature, energy conservation and consumption reduction;
(4) the reaction temperature of the reactants is accurately regulated and controlled by a heating device in a specific reaction interval, so that a target product with higher purity can be obtained more conveniently, the temperature is automatically raised and maintained in the process, the reactants do not need to be pushed repeatedly, and the external interference is greatly reduced;
(5) semi-continuous production, the first ceramic boat is immediately transferred to a circulating water cooling area after the reaction at the central position of a hearth is finished, the second ceramic boat filled with solid-phase reactants immediately enters the hearth for reaction, the previous batch of products are subjected to heat preservation reaction while being cooled (the cooled products are still in an ammonia atmosphere and can continue to react), the previous batch of products are cooled and treated well after the new products are reacted, seamless connection is realized, repeated opening times and idle time of the device are greatly avoided, and the purpose of continuously synthesizing a large amount of BNNTs is realized.
Drawings
FIG. 1 is a schematic view of the overall structure of the apparatus of the present invention;
FIG. 2 is a sectional view (lower half) of a circulating water tray at the head or tail of the furnace of the present invention;
FIG. 3 is an XDR map of BNNTs prepared in example 2 of the present invention;
FIG. 4 is a Raman spectrum of BNNTs prepared in example 2 of the present invention;
FIG. 5 is a TEM image of BNNTs prepared in example 2 of the present invention.
The furnace comprises an A-electric control heating device, a B-furnace body, a C-furnace head, a D-furnace tail, a 1-furnace head exhaust pipe, a 2-furnace tail air inlet pipe, a 3-furnace head furnace door, a 4-furnace tail furnace door, a 5-furnace head sealing cover, a 6-furnace tail sealing cover, a 7-furnace shell, an 8-furnace chamber, a 9-furnace lining, a 10-heat preservation layer, an 11-furnace head table, a 12-furnace tail table, a 13-stainless steel pipe, a 14-furnace tube, a 15-1 furnace head circulating water support, a 15-2 furnace tail circulating water support, a 16-flange, a 17-stainless steel protective cover and an 18-adjusting base.
Detailed Description
In order to make those skilled in the art fully understand the technical solutions and advantages of the present invention, the following description is given with reference to specific examples.
Example 1
The method for synthesizing the boron nitride nanotube with smooth inner wall by using the equipment shown in figure 1 provided by the invention comprises the following steps:
the advance check ensures that the whole equipment is well-functioning. Starting the electric control heating device A, setting the temperature to heat the hearth 8, and enabling the heating rate to be 4-8 ℃/min. Closing the furnace end furnace door 3 and the furnace tail furnace door 4, opening the furnace end exhaust pipe 1 and the furnace tail gas inlet pipe 2, vacuumizing and exhausting the hearth 8, continuously conveying ammonia gas into the hearth 8 through the furnace tail gas inlet pipe 2, controlling the flow of the ammonia gas to be 0.4-1.0L/min, and keeping the pipeline gas circulator in an open working state. And then placing the ceramic boat fully paved with the superfine boron carbide powder into a hearth 8 of a furnace body B for heat preservation reaction at the reaction temperature of 900-1350 ℃ for 10-15 h. And after the reaction is finished, opening a furnace end furnace door 3 of the furnace end C, moving the ceramic boat to a cooling area between the furnace body B and the furnace tail D by using a push rod for annealing, and simultaneously putting the other ceramic boat which is fully paved with boron carbide powder into a hearth for heat preservation and reaction. And repeating the steps to continuously and uninterruptedly carry out the reaction. During the period, the annealed ceramic boat is taken out through a furnace tail furnace door 4 of a furnace tail D, and the obtained product is subjected to acid washing, water washing, filtering and drying treatment to obtain the boron nitride nanotube with smooth inner wall.
Example 2
The method for synthesizing the bamboo-joint-type boron nitride nanotube by using the equipment shown in the figure 1 provided by the invention is basically similar to the method of the embodiment 1, and the difference is that: the heating rate is 6-10 ℃/min, the ammonia gas flow is 0.6-1.2L/min, the heat preservation temperature is 900-. XRD, Raman spectrum and TEM analysis of the bamboo-type BNNTs obtained in example 2 are shown in FIGS. 3-5.
As can be seen from the characteristic XRD diffraction pattern of the BNNTs sample in figure 3, the characteristic diffraction peaks are very clear, which indicates that the sample has better crystallization degree. Wherein the d-values of the characteristic diffraction peaks are at 0.33492, 0.21843, 0.20786 and 0.16693nm, corresponding to the (002), (100), (101) and (004) crystal planes of hexagonal boron nitride, respectively. The cell constants of the product are calculated to be a-0.2510 nm and c-0.6766 nm, which basically correspond to a-0.2504 nm and c-0.6661 nm in the standard card JCPDF 73-2095 of hexagonal boron nitride, and the obtained product is the hexagonal boron nitride. In addition, no peak of B4C which is not completely reacted is found in the XRD pattern, which indicates that the raw material B4C is completely reacted.
FIG. 4 is a Raman spectrum of a BNNTs sample. 1360cm-1Nearby absorption peak and E of hexagonal boron nitride network structure2g, corresponding in-plane vibration modes; in addition, other characteristic absorption peaks do not appear in the Raman spectrum, and the sample component is high-purity hexagonal boron nitride.
From the TEM photograph of fig. 5, it can be observed that the nanotube is periodically changed in a bamboo-like manner, the outer wall of the nanotube is smooth, the inner hollow structure is tapered, and the outer diameter is about 200 nm.
Claims (8)
1. A preparation method of a boron nitride nanotube is characterized by comprising the following steps:
(a) firstly, starting an electric control heating device A, and setting the temperature to heat a hearth (8) of a furnace body B;
(b) then closing a furnace end furnace door (3) and a furnace tail furnace door (4), opening a furnace end exhaust pipe (1) and a furnace tail gas inlet pipe (2), vacuumizing a hearth (8) to exhaust air as far as possible, continuously conveying ammonia gas into the hearth (8) through the furnace tail gas inlet pipe (2), and then putting the ceramic boat fully paved with boron carbide powder into the hearth (8) for heat preservation reaction; wherein the flow rate of ammonia gas is 0.4-1.2L/min, the heating rate of the hearth is 4-10 ℃/min, the ceramic boat fully paved with boron carbide powder is heated to 900-;
(c) after the reaction is finished, opening a furnace end furnace door (3) of the furnace end C, moving the ceramic boat to a cooling area between the furnace body B and the furnace tail D by using a push rod for annealing, and simultaneously putting the other ceramic boat fully paved with boron carbide powder into a hearth (8) for reaction;
(d) repeating the step (c), taking out the annealed ceramic boat through a furnace tail furnace door (4) of a furnace tail D, soaking the obtained product in 10-20 wt% HCl solution for 8-16h, filtering and washing the product until filtrate is neutral, and finally placing the filter cake in an environment at 60-90 ℃ for 8-16h to obtain the boron nitride nanotube;
the preparation furnace used in the preparation process comprises an electric control heating device A, a furnace body B, a furnace head C, a furnace tail D and a push rod; the electric control heating device A is fixed on the furnace body B and is used for heating the furnace body B under a controlled condition; a furnace end exhaust pipe (1) and a furnace end furnace door (3) are arranged on the furnace end C, and a furnace tail air inlet pipe (2) and a furnace tail furnace door (4) are arranged on the furnace tail D; the furnace head C and the furnace tail D are communicated with a hearth (8) in the furnace body B through a furnace tube (14) to form a complete gas inlet and outlet channel; the push rod can enter a hearth (8) of the furnace body B through the furnace head C and the furnace tube (14) and push a product in the hearth to the furnace tube between the furnace tail D and the furnace body B.
2. The method of claim 1, wherein: the electric control heating device A comprises an electric control cabinet and a heating element, and the electric control cabinet can control the heating element to heat and raise the temperature of the furnace body B according to a set program, so that the temperature in the hearth is stabilized at a set value.
3. The method of claim 1, wherein: furnace body B includes stove outer covering (7), furnace (8), furnace lining (9), heat preservation (10), and it has furnace lining (9) to set up to wrap up around furnace (8) inside furnace body B, and it has heat preservation (10) and stove outer covering (7) to wrap up outside furnace lining (9), and stove outer covering (7) adopt double-deck forced air cooling structure.
4. The method of claim 1, wherein: the furnace end C comprises a furnace end exhaust pipe (1), a furnace end furnace door (3), a furnace end sealing cover (5), a furnace end table (11) and a furnace end circulating water support (15-1); the furnace end exhaust pipe (1) is communicated with the furnace tube (14) and is used for vacuumizing and exhausting waste gas in the hearth; a furnace end circulating water support (15-1) is sleeved on the outer surface of the furnace tube (14), one end of the furnace end circulating water support is fixed on the furnace end table (11), and the other end of the furnace end circulating water support is fixed on the furnace body B; the furnace end sealing cover (5) wraps the furnace end table (11) and the furnace end circulating water support (15-1) and seals the furnace end table and the furnace end circulating water support; the furnace end exhaust pipe (1) is arranged on the furnace end sealing cover (5), and the furnace end furnace door (3) is arranged at the end part of the furnace tube (14).
5. The method of claim 1, wherein: the furnace tail D comprises a furnace tail air inlet pipe (2), a furnace tail sealing cover (6), a furnace tail furnace door (4), a furnace tail table (12) and a furnace tail circulating water support (15-2); the furnace tail gas inlet pipe (2) is communicated with the furnace tube (14) and is used for conveying feed gas ammonia gas into the hearth; a furnace tail circulating water support (15-2) is sleeved on the outer surface of the furnace tube (14) to form a cooling area, one end of the furnace tail circulating water support (15-2) is fixed on the furnace tail table (12), and the other end of the furnace tail circulating water support is fixed on the furnace body B; the furnace tail sealing cover (6) wraps the furnace tail table (12) and the furnace tail circulating water support (15-2) and seals the furnace tail table and the furnace tail circulating water support; the furnace tail gas inlet pipe (2) is arranged on the furnace tail sealing cover (6), and the furnace tail furnace door (4) is arranged at the end part of the furnace tube (14).
6. The method of claim 5, wherein: stainless steel pipes (13) and stainless steel protective covers are arranged on the outer surfaces of the furnace tail circulating water support (15-1) and the furnace head circulating water support (15-2), adjusting bases (18) are arranged at the bottoms of the furnace head table (11) and the furnace tail table (12), and the furnace tail circulating water support, the furnace head circulating water support and the cooling water phase are arranged.
7. The method of claim 1, wherein: a gas circulating device is also arranged between the furnace end exhaust pipe (1) and the furnace tail gas inlet pipe (2).
8. The furnace used for the method of producing boron nitride nanotubes according to claim 1, characterized in that: the furnace comprises an electric control heating device A, a furnace body B, a furnace head C, a furnace tail D and a push rod; the electric control heating device A is fixed on the furnace body B and is used for heating the furnace body B under a controlled condition; a furnace end exhaust pipe (1) and a furnace end furnace door (3) are arranged on the furnace end C, and a furnace tail air inlet pipe (2) and a furnace tail furnace door (4) are arranged on the furnace tail D; the furnace head C and the furnace tail D are communicated with a hearth (8) in the furnace body B through a furnace tube (14) to form a complete gas inlet and outlet channel; the push rod can enter a hearth (8) of the furnace body B through the furnace head C and the furnace tube (14) and push a product in the hearth to the furnace tube between the furnace tail D and the furnace body B.
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| CN1840266A (en) * | 2006-01-26 | 2006-10-04 | 湖南凯丰新材料有限公司 | Preparation method and equipment for nano-grade superfine cobalt powder |
| CN101885477A (en) * | 2010-07-15 | 2010-11-17 | 武汉工程大学 | Boron nitride nanotube synthesizer |
| CN102351208A (en) * | 2011-07-08 | 2012-02-15 | 武汉工程大学 | Method for rapidly producing boron nitride by using intermediate frequency carbon tube furnace |
| CN207779120U (en) * | 2018-01-19 | 2018-08-28 | 赣州力信达冶金科技有限公司 | A kind of carbon shirt-circuiting furnace |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2002289616A (en) * | 2001-03-28 | 2002-10-04 | Mitsubishi Heavy Ind Ltd | Method and apparatus for forming film |
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|---|---|---|---|---|
| CN1840266A (en) * | 2006-01-26 | 2006-10-04 | 湖南凯丰新材料有限公司 | Preparation method and equipment for nano-grade superfine cobalt powder |
| CN101885477A (en) * | 2010-07-15 | 2010-11-17 | 武汉工程大学 | Boron nitride nanotube synthesizer |
| CN102351208A (en) * | 2011-07-08 | 2012-02-15 | 武汉工程大学 | Method for rapidly producing boron nitride by using intermediate frequency carbon tube furnace |
| CN207779120U (en) * | 2018-01-19 | 2018-08-28 | 赣州力信达冶金科技有限公司 | A kind of carbon shirt-circuiting furnace |
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