CN113416086A - Rotary furnace carbon ceramic furnace tube for CVD carbon vapor deposition, rotary furnace and preparation method of carbon ceramic furnace tube - Google Patents
Rotary furnace carbon ceramic furnace tube for CVD carbon vapor deposition, rotary furnace and preparation method of carbon ceramic furnace tube Download PDFInfo
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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Abstract
The invention discloses a rotary furnace carbon ceramic furnace tube for CVD carbon vapor deposition, a rotary furnace and a preparation method of the carbon ceramic furnace tube. The preparation method of the carbon ceramic furnace tube comprises the following steps: alternately stacking a plurality of layers of carbon fiber laid fabrics and carbon fiber net tires, and performing needling composite to form a tubular structure, wherein the tubular structure is subjected to thermosetting treatment and chemical vapor deposition to obtain a furnace tube blank; machining the blank to obtain a finish-machined furnace tube blank; and carrying out melting siliconizing treatment and carbonization siliconizing treatment on the furnace tube blank for finish machining to obtain the carbon ceramic furnace tube. The carbon ceramic furnace tube has the advantages of low density, wear resistance, high strength, oxidation resistance, no heat fading and the like, particularly does not react with hydrogen and hydrocarbon organic gas to generate hydrogen embrittlement corrosion cracking, can avoid introducing metal impurities in the processing process of a silicon-based negative electrode material, and can be widely applied to high-temperature furnace tubes of various processes such as CVD carbon vapor deposition, cladding, ammonia decomposition of hydrogen and the like.
Description
Technical Field
The invention relates to a rotary furnace tube and a preparation method thereof, in particular to a rotary furnace carbon ceramic tube for CVD carbon vapor deposition and a preparation method thereof, and also relates to a rotary furnace for CVD carbon vapor deposition, which comprises the carbon ceramic tube, and belongs to the technical field of CVD carbon vapor deposition.
Background
With the rapid development of electric vehicles, energy storage power stations, portable electronic devices, and the like, lithium ion batteries with high specific energy are receiving more and more attention.
However, the graphite cathode still firmly occupies the dominating position at present, the theoretical specific capacity of the graphite cathode is 372mAh/g, the requirement of a high-specific-energy battery cathode material cannot be met, and the improvement of the energy density of a lithium battery is severely restricted.
Scientists around the world have been trying to develop negative electrode materials such as silicon-based negative electrode materials, tin-based materials, and lithium titanate materials that can replace graphite for many years. And the silicon or silicon-oxygen cathode material is the only new high-capacity cathode material for commercial application at present.
At present, the mainstream commercial silicon monoxide composite negative electrode material is generally coated with carbon, so that on one hand, the conductivity of the material is improved, the volume expansion of the silicon after lithium insertion is reduced, meanwhile, the direct contact of the silicon monoxide material and electrolyte is also avoided, and the cycle performance of the material is improved.
The CVD carbon gas phase coating silicon or silicon-oxygen lithium battery negative electrode material is generally realized by adopting a rotary furnace, the working temperature is about 1000 ℃, and the outer wall of the furnace tube of the rotary furnace is exposed in the air, so that high-temperature oxidation is easily caused. The diameter of the furnace tube of the prior rotary furnace is more than 300 mm, the length of the furnace tube exceeds 4000mm, the furnace tube needs to bear certain impact and larger torque during rotation, quartz and conventional ceramic materials can not meet the operating requirements of working conditions, and the furnace tube of the rotary furnace is generally made of heat-resistant stainless steel materials at the present stage. The technical problem that the hydrogen embrittlement is easy exists in the steel material, for example ("physical test", 2 nd, 1994) reports that austenitic stainless steel has a serious hydrogen embrittlement tendency, and ("general corrosion control", 29 th volume, 08 th period, 2015 08 th month) also shows that the diffusion coefficient of hydrogen in martensite is two orders of magnitude higher than that in austenite, the hydrogen diffuses rapidly, the brittleness of martensitic stainless steel is higher than that of austenitic stainless steel, hydrogen induced stress corrosion cracking is caused, particularly, the content of metal impurities required for processing a silicon-based anode material is extremely low, and the stainless steel is easy to introduce the metal impurities of the silicon anode material.
In conclusion, the problem to be solved by the technical personnel in the field is how to solve the defects that the CVD carbon vapor deposition rotary furnace tube has poor oxidation resistance, is easy to cause hydrogen embrittlement, is easy to introduce metal impurities and the like, and meets the requirement of a silicon or silicon-based negative electrode carbon coating process.
Disclosure of Invention
The first objective of the present invention is to provide a carbon ceramic furnace tube for a rotary furnace used for CVD carbon vapor deposition, which has the advantages of low density, wear resistance, high strength, oxidation resistance, no heat fading, etc., and particularly, the carbon ceramic furnace tube does not react with hydrogen gas and hydrocarbon organic gas to generate hydrogen embrittlement corrosion cracking, can avoid introducing metal impurities in the processing process of silicon-based negative electrode materials, and can be widely applied to various high temperature furnace tubes for CVD carbon vapor deposition, cladding, ammonia decomposition hydrogen, etc.
The second purpose of the invention is to provide a preparation method of a carbon ceramic furnace tube of a rotary furnace for CVD carbon vapor deposition, which has simple steps and low cost and is beneficial to large-scale production.
The third purpose of the invention is to provide a rotary furnace for CVD carbon vapor deposition, which uses a furnace tube made of carbon ceramic material, can meet the process requirement of silicon or silicon-based cathode carbon coating, and solves the technical problems of poor oxidation resistance, easy hydrogen embrittlement, easy introduction of metal impurities and the like of the existing stainless steel material furnace tube.
In order to achieve the technical purpose, the invention provides a preparation method of a carbon ceramic furnace tube of a rotary furnace for CVD carbon vapor deposition, which comprises the following steps:
1) alternately stacking a plurality of layers of carbon fiber laid cloth and a carbon fiber net tire, and performing needling composite to form a tubular structure, wherein the tubular structure is subjected to thermosetting treatment to obtain a carbon fiber preform;
2) carrying out chemical vapor deposition on the carbon fiber preform to obtain a furnace tube blank;
3) machining the blank to obtain a finish-machined furnace tube blank;
4) and carrying out melting siliconizing treatment and carbonization siliconizing treatment on the furnace tube blank for finish machining to obtain the finished product.
As an optimal scheme, the total number of the carbon fiber non-woven cloth and the carbon fiber net tire is 14-16, and the needling density is 25-30 needles/cm3. The carbon fiber preform is mainly formed by superposing and needling carbon fiber laid cloth and a carbon fiber net tire, wherein the carbon fiber laid cloth mainly provides mechanical strength support, the carbon fiber net tire comprises a large number of chopped fibers vertical to the surface, and the chopped fibers in the net tire are penetrated into the carbon fiber laid cloth on the upper surface and the lower surface in a relay needling mode to play a riveting role, so that the bonding strength between any two layers of carbon fiber laid cloth is improved, the carbon fiber laid cloth and the carbon fiber net tire are superposed to form a whole, and the carbon fiber preform with better mechanical property is obtained. Further preferably, the carbon fiber non-woven cloth can be unidirectional or intersection non-woven cloth.
Preferably, the density of the carbon fiber preform is 0.4-0.6 g/cm3。
As a preferable mode, the conditions of the heat curing treatment are as follows: the temperature is 200-300 ℃, and the time is 5-15 h. The heat curing process mainly utilizes the residual macromolecules on the surface of the carbon fibers to carry out consolidation forming.
As a preferred scheme, the chemical vapor deposition comprises a pretreatment process and an isothermal isobaric chemical vapor deposition process; the conditions of the pretreatment process are as follows: the temperature is 950-1100 ℃, natural gas and/or ethylene are/is used as a gas carbon source, nitrogen is used as carrier gas, the flow rate of the gas carbon source is 40-80L/min, and the deposition time is 100-200 h; the isothermal isobaric chemical vapor deposition conditions are as follows: the temperature is 950-1100 ℃, natural gas and/or ethylene are/is used as a gas carbon source, nitrogen is used as carrier gas, the flow rate of the gas carbon source is 40-80 l/min, and the deposition time is 100-200 h. After the carbon fiber preform is pretreated, the obtained blank is processed to be in a proper size, the length of the blank is processed in place, the inner diameter and the outer diameter of the blank are respectively reserved for 5cm, and then the subsequent isothermal and isobaric chemical vapor deposition is carried out.
As a preferable scheme, silicon powder is sprayed on the surface of a finish machining furnace tube blank, and is subjected to melting siliconizing treatment for 1-5 hours at the temperature of 1600-1800 ℃ and then to carbonization siliconizing treatment for 0.5-2 hours at the temperature of 1600-1800 ℃. Silicon powder is sprayed on the upper surface and the lower surface of the carbon fiber preform, silicon is firstly melted under the action of high temperature and permeates into the carbon fiber material under the capillary action, and then the silicon and matrix carbon react at the high temperature to obtain the C/C-SiC composite material. And repeating the melting siliconizing treatment and the carbonization siliconizing treatment on the furnace tube blank for multiple times according to actual needs.
As a preferable scheme, the mass of the silicon powder is 1/5-1/2 of the mass of the blank of the finish machining furnace tube.
The carbon fiber preform can be formed by a mold, for example, a cylindrical foam model is utilized, the outer diameter of the cylindrical foam model is smaller than the inner diameter of the existing stainless steel furnace pipe, the length of the cylindrical foam model is larger than the length of the existing stainless steel furnace pipe, the laid cloth and the net tire are alternately subjected to cyclic layering on the surface of the cylindrical foam model, needling lamination is carried out on every two layers until the required thickness is reached, and then thermocuring treatment is carried out. The outer diameter of the cylindrical foam model is smaller than the inner diameter of the carbon ceramic furnace tube by 1-2 cm, the length of the cylindrical foam model is larger than the length of the carbon ceramic furnace tube by 4cm, the outer diameter of the carbon fiber tubular preform is larger than the finished carbon ceramic furnace tube of the rotary furnace by 1-2 cm, and the excess length of the carbon fiber tubular preform is cut off in the subsequent machining process.
The invention also provides a rotary furnace carbon ceramic furnace tube for CVD carbon vapor deposition, which is obtained by the preparation method.
The invention also provides a rotary furnace for CVD carbon vapor deposition, which comprises the carbon ceramic furnace tube.
As a preferable scheme, the carbon ceramic furnace tube is wound on the inner side of the stainless steel furnace tube of the rotary furnace.
As a preferable scheme, an L-shaped spiral material guide plate is arranged on the inner wall of the carbon ceramic furnace tube. The L-shaped spiral material guide plate is mainly used for controlling the flow of materials in the furnace pipe and preventing material return.
The carbon ceramic furnace tube has a circular section, the surface roughness of the carbon ceramic furnace tube meets 0.8< Ra <1, the specification of the carbon ceramic furnace tube is phi 400 x 5000mm in outer diameter (specifically, the outer diameter of the carbon ceramic furnace tube is slightly smaller than the inner diameter of the stainless steel furnace tube according to the setting of the existing stainless steel furnace tube so as to be convenient for installation), and the wall thickness of the carbon ceramic furnace tube is 12 mm. The carbon ceramic furnace tube is in direct contact with the material, and the front section of the inner wall is provided with an L-shaped spiral material guide plate to prevent material returning. The middle high-temperature section can also be provided with a material turning plate and an L-shaped material raising plate which are the same as the material turning plate and the L-shaped material raising plate arranged in the existing stainless steel furnace pipe, and the material turning plate and the L-shaped material raising plate are arranged conventionally, so that the material can be fully contacted with reaction gas and can move axially and radially, the materials on the upper layer and the lower layer can be heated uniformly and alternately, and the heating is uniform.
The key improvement of the rotary furnace for CVD carbon vapor deposition is that the carbon ceramic furnace tube made of special materials is designed, the existing rotary furnace is not required to be adjusted greatly, the carbon ceramic furnace tube is only required to be added on the inner wall of the heat-resistant stainless steel furnace tube, and a conventional L-shaped spiral guide plate, a material turning plate, an L-shaped material raising plate and the like in the furnace tube are arranged in the carbon ceramic furnace tube.
The rotary furnace commonly used for CVD carbon vapor deposition in the prior art comprises a rotary furnace tube, a furnace body frame, a heating group section and the like. The furnace body frame is divided into an upper layer and a lower layer, and the upper layer and the lower layer are partially welded, and the furnace body frame is made of stainless steel, section steel, steel plates and the like which are correspondingly resistant to high-temperature gas medium corrosion according to the medium property of a corrosion working condition. The upper layer of the furnace body frame is mainly used for placing a heating furnace body, and the lower layer of the furnace body frame is used for placing transmission systems such as furnace body angle adjustment accessories and the like. The safety shield plate of the heating furnace body shell is composed of steel plates and is formed by stamping, shearing, folding and welding cold plates. The fire-resistant layer at the bottom of the heating furnace body is made of high-quality refractory bricks and light bricks, the heating elements are Cr27Al7Mo2 type high-temperature resistance wires, the heat-insulating layers on the two sides are high-temperature-resistant ceramic fiber plates, and the heating elements are arranged in the heat-insulating modules on the two sides. The furnace body angular adjustment system is installed to heating furnace body bottom, can supply to go up and down to this inclination of adjusting the furnace body makes the material slowly roll from the feed end to the discharge end under the effect of gravity, runs through whole furnace body. The furnace tube sealing adopts graphite machinery and air ring combined sealing, the stone mill mechanical sealing adopts a domestic leading automatic compensation wall graphite ring sealing mode, the sealing performance is good, air and powder leakage are avoided, the maintenance is easy, the air ring sealing adopts an air source, a multi-point air inlet mode is adopted, a nitrogen sealing atmosphere is formed on a sealing surface, the furnace atmosphere is isolated from the outside air, the overflow of the furnace gas and the entrance of the outside air are avoided, and the safe and stable operation of the equipment is ensured. The furnace cover of the heating furnace body is of an opening and closing structure, and the furnace cover heat preservation layer is assembled by adopting high-temperature ceramic fiber modules. Two sets of mechanical rapping devices are respectively arranged at two ends of the heating furnace body and are used for slowing down the phenomenon that materials in the roller are stuck to the wall. The furnace body length of the heating group section is about 4000mm, the length of each zone is 660mm, the heating is carried out in 6 zones, the heating power of each zone is 15KW, and the heating power can be independently controlled; the temperature measuring elements are K-type thermocouples and are inserted from the side wall of the hearth, and the number of the temperature measuring elements is 6; the heating element is a Cr27Al7Mo2 type high-temperature resistance wire. The rotary tube furnace tube is made of Japan imported heat-resistant stainless steel 310S, the section is circular, and the surface roughness is 0.8< Ra < 1; the outside diameter was 400 x 5000mm, and the tube wall thickness was 12 mm. The front section of the inner wall of the inner roller of the furnace tube is provided with a spiral material guide plate, and the high-temperature section is provided with a material turning plate and an L-shaped material raising plate.
The structure sketch of the rotary furnace device of the invention is shown in figure 1, and the main body comprises a feeding bin 1, a feeder 2, an exhaust pipeline 3, a furnace body angle adjusting accessory 4, a heating furnace body 5, a rotary drum furnace tube 6 and a discharging bin 7. The feeding bin 1 is connected with a quantitative screw feeder 2 and is connected with a rotary drum furnace tube 6. The exhaust pipeline 3 is responsible for controlling the vacuum environment in the furnace, and the furnace body angle adjusting accessory 4 adjusts the height of the discharge end at the feed end of the furnace body, so that the material moves under the action of gravity. The heating furnace body 5 is responsible for improving the heating of the revolving furnace tube 6. Referring to fig. 4, the L-shaped spiral guide plate in the furnace tube 6 of the revolving drum stirs and mixes the materials during the heating process, so as to ensure that the materials are heated uniformly and react sufficiently, and finally, the discharging is completed through the discharging bin 7 under the action of the gravity of the spiral guide plate.
Compared with the prior art, the technical scheme of the invention has the following beneficial technical effects:
the carbon ceramic furnace tube for the CVD carbon vapor deposition rotary furnace provided by the invention has the advantages of low density, wear resistance, high strength, oxidation resistance, no heat fading and the like, and the carbon ceramic furnace tube is applied to the rotary furnace, so that the hydrogen embrittlement reaction caused by the existing stainless steel furnace tube can be effectively solved only by winding the carbon ceramic furnace tube around and arranging the carbon ceramic furnace tube at the inner side of the common high-temperature resistant stainless steel rotary furnace tube without greatly improving the existing rotary furnace, and the extremely low metal impurity content required by a silicon-based cathode process can be met to the greatest extent.
The preparation method of the rotary furnace carbon ceramic furnace tube for CVD carbon vapor deposition is simple, low in cost and beneficial to large-scale production.
Drawings
FIG. 1 is a schematic view of a rotary kiln apparatus; wherein, 1 is a feeding bin, 2 is a feeder, 3 is an exhaust pipeline, 4 is a furnace body angle adjusting accessory, 5 is a heating furnace body, 6 is a rotary drum furnace tube, and 7 is a discharging bin.
FIG. 2 is an electron micrograph of silicon monoxide after CVD carbon gas phase coating in a conventional rotary kiln.
FIG. 3 is an electron microscope image of silicon monoxide after CVD carbon gas phase coating in a rotary furnace equipped with a carbon ceramic furnace tube.
FIG. 4 is a schematic view of the interior of a carbon ceramic furnace tube.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The carbon fiber laid fabric and the carbon fiber mesh tire referred to in the embodiment are common commercial products in the market.
Example 1
1) The carbon fiber non-woven fabric and the carbon fiber net tire are alternately overlapped, a cylindrical foam model is utilized, the outer diameter of the cylindrical foam model is smaller than the inner diameter of the carbon ceramic furnace tube by 1cm, the length of the cylindrical foam model is larger than the length of the carbon ceramic furnace tube by 4cm, the outer diameter of the carbon fiber tubular preform is larger than the finished carbon ceramic furnace tube of the rotary furnace by 1cm, and the excess length is cut off in the subsequent machining process. And (3) alternately performing circulating layering on the surface of the cylindrical foam model by using the non-woven cloth and the net tire, and stacking 16 layers. Needling every two layers at 30 needles/cm3The tubular structure is compositely formed by needling density, and is thermally cured at 300 ℃ for 15hTreated to obtain 0.6g/cm3A carbon fiber preform.
2) Carrying out chemical vapor deposition on the carbon fiber preform, wherein the chemical vapor deposition comprises a primary pretreatment process and a primary isothermal and isobaric chemical vapor deposition process; the conditions of the pretreatment process are as follows: the temperature is 950 ℃, natural gas is used as a gas carbon source, nitrogen is used as carrier gas, the flow rate of the gas carbon source is 40 liters/minute, and the deposition time is 100 hours; the isothermal isobaric chemical vapor deposition conditions are as follows: the temperature is 1100 ℃, ethylene is used as a gas carbon source, nitrogen is used as a carrier gas, the flow rate of the gas carbon source is 80 liters/minute, and the deposition time is 200 hours, so that the furnace tube blank is obtained.
3) The obtained furnace tube blank is subjected to finish machining to obtain a furnace tube blank with the inner diameter of 400mm, the length of 5000mm and the inner and outer diameters of 50mm respectively, so that the finish machining furnace tube blank is obtained.
4) The silicon powder of 1/3 with the quality of the blank body of the finishing furnace tube is sprayed on the surface of the blank body of the finishing furnace tube, and is firstly subjected to melting siliconizing treatment for 1h at the temperature of 1650 ℃, and then is subjected to carbonization siliconizing treatment for 1h at the temperature of 1800 ℃.
The bending strength of the prepared carbon ceramic furnace tube is 133MPa, the fracture strain is about 1.3 percent, and the fracture toughness is 9MPa m1 /2。
Example 2
1) The carbon fiber non-woven fabric and the carbon fiber net tire are alternately overlapped, a cylindrical foam model is utilized, the outer diameter of the cylindrical foam model is smaller than the inner diameter of the carbon ceramic furnace tube by 1cm, the length of the cylindrical foam model is larger than the length of the carbon ceramic furnace tube by 4cm, the outer diameter of the carbon fiber tubular preform is larger than the finished carbon ceramic furnace tube of the rotary furnace by 1cm, and the excess length is cut off in the subsequent machining process. And (3) alternately performing circulating layering on the surface of the cylindrical foam model by using the non-woven cloth and the net tire, and stacking 16 layers. Needling every two layers at 30 needles/cm3The tubular structure is formed by compounding needling density, and is thermally cured at 300 ℃ for 15 hours to obtain 0.6g/cm3A carbon fiber preform.
2) Carrying out chemical vapor deposition on the carbon fiber preform, wherein the chemical vapor deposition comprises a primary pretreatment process and a primary isothermal and isobaric chemical vapor deposition process; the conditions of the pretreatment process are as follows: the temperature is 950 ℃, natural gas is used as a gas carbon source, nitrogen is used as carrier gas, the flow rate of the gas carbon source is 40 liters/minute, and the deposition time is 100 hours; the isothermal isobaric chemical vapor deposition conditions are as follows: the temperature is 1100 ℃, ethylene is used as a gas carbon source, nitrogen is used as a carrier gas, the flow rate of the gas carbon source is 80 liters/minute, and the deposition time is 200 hours, so that the furnace tube blank is obtained.
3) The obtained furnace tube blank is subjected to finish machining to obtain a furnace tube blank with the inner diameter of 400mm, the length of 5000mm and the inner and outer diameters of 50mm respectively, so that the finish machining furnace tube blank is obtained.
4) The silicon powder of 1/3 with the quality of the blank body of the finishing furnace tube is sprayed on the surface of the blank body of the finishing furnace tube, and is firstly subjected to melting siliconizing treatment for 2 hours at the temperature of 1650 ℃, and then is subjected to carbonization siliconizing treatment for 1 hour at the temperature of 1800 ℃. Thus obtaining the carbon ceramic furnace tube.
The bending strength of the prepared carbon ceramic furnace tube is 101MPa, the fracture strain is about 1.4 percent, and the fracture toughness is 9MPa m1 /2。
Example 3
1) The carbon fiber non-woven fabric and the carbon fiber net tire are alternately overlapped, a cylindrical foam model is utilized, the outer diameter of the cylindrical foam model is smaller than the inner diameter of the carbon ceramic furnace tube by 1cm, the length of the cylindrical foam model is larger than the length of the carbon ceramic furnace tube by 4cm, the outer diameter of the carbon fiber tubular preform is larger than the finished carbon ceramic furnace tube of the rotary furnace by 1cm, and the excess length is cut off in the subsequent machining process. And (3) alternately performing circulating layering on the surface of the cylindrical foam model by using the non-woven cloth and the net tire, and stacking 16 layers. Needling every two layers at 30 needles/cm3The tubular structure is formed by compounding needling density, and is thermally cured at 300 ℃ for 15 hours to obtain 0.6g/cm3A carbon fiber preform.
2) Carrying out chemical vapor deposition on the carbon fiber preform, wherein the chemical vapor deposition comprises a primary pretreatment process and a primary isothermal and isobaric chemical vapor deposition process; the conditions of the pretreatment process are as follows: the temperature is 950 ℃, natural gas is used as a gas carbon source, nitrogen is used as carrier gas, the flow rate of the gas carbon source is 40 liters/minute, and the deposition time is 100 hours; the isothermal isobaric chemical vapor deposition conditions are as follows: the temperature is 1100 ℃, ethylene is used as a gas carbon source, nitrogen is used as a carrier gas, the flow rate of the gas carbon source is 80 liters/minute, and the deposition time is 200 hours, so that the furnace tube blank is obtained.
3) The obtained furnace tube blank is subjected to finish machining to obtain a furnace tube blank with the inner diameter of 400mm, the length of 5000mm and the inner and outer diameters of 50mm respectively, so that the finish machining furnace tube blank is obtained.
4) The silicon powder of 1/3 with the quality of the blank body of the finishing furnace tube is sprayed on the surface of the blank body of the finishing furnace tube, and is firstly subjected to melting siliconizing treatment for 5 hours at the temperature of 1650 ℃, and then is subjected to carbonization siliconizing treatment for 1 hour at the temperature of 1800 ℃. And (5) obtaining the product.
The bending strength of the prepared carbon ceramic furnace tube is 86MPa, the fracture strain is about 1.5 percent, and the fracture toughness is 8MPa m1 /2。
Application examples
The carbon ceramic furnace tube prepared in the specific example 2 is installed on the inner wall of the high-temperature resistant stainless steel furnace tube of the NMIHY-R40L500-6 rotary furnace, and the rotary furnace provided with the carbon ceramic furnace tube and the conventional common rotary furnace carry out CVD carbon gas phase coating on the silicon monoxide under the same condition.
The specific process comprises the following steps: the equipment adopts an electric heating external heating rotary furnace structure, the continuous rotary motion of the furnace tube with a certain inclination angle drives the loose materials of the silica powder to do turnover spiral linear motion in the furnace tube through the rotation of the heat-resistant steel furnace tube, and the heating temperature rise process of the product is realized through a heating temperature control section arranged in a heating cavity of the furnace body; the CVD deposition has the following specific process parameters: the temperature is controlled at 880 ℃, the working gas is acetylene, and the gas flow is set to be 3m3And h, the carrier gas is argon, the material is in full contact with a carbon source generated by acetylene in the furnace, and the reaction is carried out for 3.5 hours, so that the purpose of uniformly coating the carbon source on the surface of the material is achieved.
The content of metal impurities in the silicon oxide negative electrode material formed by CVD carbon gas phase coating of the silicon oxide by adopting a common rotary furnace is as follows:
the content of metal impurities of the silicon oxide negative electrode material formed by carrying out CVD carbon gas phase coating on the silicon oxide by adopting a rotary furnace provided with a carbon ceramic furnace tube is as follows:
according to the data in the table, the content of metal impurities can be obviously reduced when the rotary furnace provided with the carbon ceramic furnace tube is coated with the silicon oxide negative electrode material.
An electron microscope image of the silicon monoxide after CVD carbon gas phase coating by a common rotary furnace is shown in fig. 2, and an electron microscope image of the silicon monoxide after CVD carbon gas phase coating by a rotary furnace provided with a carbon ceramic furnace tube is shown in fig. 3. As shown in the figure, it can be seen that in the electron microscope image shown in FIG. 3, the particle size of the silicon oxide negative electrode material is smaller, and the crystal form is more complete.
The service life of the carbon ceramic rotary furnace tube is remarkably prolonged, the service life of a common high-temperature-resistant stainless steel furnace tube is generally 1000 furnaces, and the service life of the carbon ceramic rotary furnace tube is effectively prolonged to 1500 furnaces after the carbon ceramic furnace tube is configured.
Claims (10)
1. A preparation method of a carbon ceramic furnace tube of a rotary furnace for CVD carbon vapor deposition is characterized by comprising the following steps: the method comprises the following steps:
1) alternately stacking a plurality of layers of carbon fiber laid cloth and a carbon fiber net tire, and performing needling composite to form a tubular structure, wherein the tubular structure is subjected to thermosetting treatment to obtain a carbon fiber preform;
2) carrying out chemical vapor deposition on the carbon fiber preform to obtain a furnace tube blank;
3) machining the blank to obtain a finish-machined furnace tube blank;
4) and carrying out melting siliconizing treatment and carbonization siliconizing treatment on the furnace tube blank for finish machining to obtain the finished product.
2. The method of claim 1, wherein the method comprises the following steps: the total number of the carbon fiber laid fabric and the carbon fiber net tire is 14-16, and the needling density is 25-30 needles/cm3。
3. The method of claim 1, wherein the method comprises the following steps: the density of the carbon fiber preform is 0.4-0.6 g/cm3。
4. The method of claim 1, wherein the method comprises the following steps: the conditions of the heat curing treatment are as follows: the temperature is 200-300 ℃, and the time is 5-15 h.
5. The method of claim 1, wherein the method comprises the following steps: the chemical vapor deposition comprises a primary pretreatment process and a primary isothermal isobaric chemical vapor deposition process; the conditions of the pretreatment process are as follows: the temperature is 950-1100 ℃, natural gas and/or ethylene are/is used as a gas carbon source, nitrogen is used as carrier gas, the flow rate of the gas carbon source is 40-80L/min, and the deposition time is 100-200 h; the isothermal isobaric chemical vapor deposition conditions are as follows: the temperature is 950-1100 ℃, natural gas and/or ethylene are/is used as a gas carbon source, nitrogen is used as carrier gas, the flow rate of the gas carbon source is 40-80 l/min, and the deposition time is 100-200 h.
6. The method of claim 1, wherein the method comprises the following steps: spraying silicon powder on the surface of a finish machining furnace tube blank, carrying out melt siliconizing treatment for 1-5 h at the temperature of 1600-1800 ℃, and carrying out carbonization siliconizing treatment for 0.5-2 h at the temperature of 1600-1800 ℃; the mass of the silicon powder is 1/5-1/2 of the mass of the blank of the finish machining furnace tube.
7. A rotary furnace carbon ceramic furnace tube for CVD carbon vapor deposition is characterized in that: the preparation method of any one of claims 1 to 6.
8. A rotary furnace for CVD carbon vapor deposition, characterized by: comprising the carbon ceramic tube of claim 7.
9. The rotary furnace for CVD carbon vapor deposition of claim 8, wherein: the carbon ceramic furnace tube is arranged at the inner side of the stainless steel furnace tube of the rotary furnace in a winding way.
10. The rotary furnace for CVD carbon vapor deposition of claim 9, wherein: and an L-shaped spiral material guide plate is arranged on the inner wall of the carbon ceramic furnace tube.
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Application publication date: 20210921 |