CN115784762B - Deposition method and deposition equipment for carbon-carbon thermal field material - Google Patents
Deposition method and deposition equipment for carbon-carbon thermal field material Download PDFInfo
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Abstract
The invention discloses a deposition method of a carbon-carbon thermal field material, which at least comprises the following steps: primary deposition: producing a plurality of preforms through a first column in a hot field region within a CVD furnace; preparing a second material column, arranging a plurality of prefabricated products in the height direction and sleeving a crucible side or an outer guide cylinder; secondary depositing, producing a plurality of semi-finished products in the hot field area through a second material column; semi-finished product processing, performing heat treatment and machining on the semi-finished product to obtain a semi-finished product with a preset size; preparing a third material column, arranging a plurality of semi-finished products with preset sizes in the height direction, sleeving a crucible side or an outer guide cylinder, and sleeving a layer of outer die; and (3) three times of deposition, and producing a finished product through a third material column in the hot field area. According to the deposition method provided by the invention, through a rapid pre-deposition and twice densification deposition mode, the density of a finished product is high, the surface hole sealing effect is good, the total process time is shortened to 240-300 h, and the energy consumption and the equipment depreciation rate are reduced. The invention also discloses a deposition device.
Description
Technical Field
The invention relates to the technical field of preparation of carbon-carbon thermal field materials, in particular to a deposition method and deposition equipment of a carbon-carbon thermal field material.
Background
Carbon-carbon thermal field materials, such as crucible sides, guide barrels, thermal insulation barrels and the like, have better thermal shock resistance, longer service life and high cost performance compared with graphite thermal field materials, and are widely applied as silicon single crystal drawing equipment in the photovoltaic or semiconductor industry.
The existing method for preparing the carbon-carbon thermal field material mainly comprises a pure CVI process and a CVI and liquid phase impregnation composite densification process, and the CVI process has the advantages of minimum damage to carbon fibers and high interface bonding strength of pyrolytic carbon and carbon fibers, so that the carbon-carbon thermal field material prepared by the pure CVI process has high mechanical strength, strong corrosion resistance and longer service life compared with the carbon-carbon thermal field material prepared by the CVI and liquid phase impregnation process under the same density.
Pure CVI processes are usually prefabricated using needlingThe body is used as a reinforcing framework to carry out multiple CVI densification and mechanical shelling cycles, wherein the needled preform is a carbon fiber preform manufactured by net tire, plain cloth and wound wire lamination needling, and the CVI process is generally divided into three types, namely a single-material-column low-layer (below 1-material-column 3-layer) isothermal isobaric CVI process, a multi-material-column low-layer (below 7-material-column 3-layer) isothermal isobaric CVI process and a multi-material-column high-layer (above 7-material-column 6-layer) isothermal isobaric CVI process, wherein the multi-material-column high-layer isothermal isobaric CVI process is generally carried out by using a vertical cylindrical chemical vapor deposition furnace (CVD furnace), the deposition cycle is 3-4 times (2-3 times of deposition and 1 time of coating), the total deposition time is 600-700 hours, the energy consumption of unit materials can be remarkably reduced by improving single-time yield, but the prepared materials have low density and low qualification rate, and the density qualification rate of secondary deposition (density is 1.30 g/cm) 3 Above) is only about 50%, the needled preform is firstly deposited to a certain density through CVI, and then impregnated and carbonized for multiple times, so that the density and density uniformity of a prepared product can be improved, but the preparation period of the material is long, usually 3-4 months, and the impregnation process has great damage to fibers, so that the mechanical property and brittleness of the product material are poor, the material cost is high, and the environmental pollution is great.
Therefore, how to ensure that the prepared carbon-carbon thermal field material has good mechanical properties, reduce the preparation process duration, reduce the unit energy consumption and the equipment depreciation rate, and is a technical problem which needs to be solved by the technicians in the field.
Disclosure of Invention
Therefore, the invention aims to provide a deposition method of a carbon-carbon thermal field material, which can ensure that the prepared carbon-carbon thermal field material has good mechanical properties, reduce the preparation process time and reduce the unit energy consumption and the equipment depreciation rate.
It is another object of the present invention to provide a deposition apparatus for a carbon-carbon thermal field material suitable for the above deposition method.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method of depositing a carbon-carbon thermal field material, comprising at least the steps of:
primary deposition: at CV Setting up a plurality of first material columns in a hot field area in a furnace D, regulating the pressure in the furnace to be not more than 300Pa, heating the bottom of the hot field area to 1145-1150 ℃ through a three-stage independent heating system arranged along the height direction of the hot field area, heating the middle part to 1135-1140 ℃ and the upper part to 1125-1130 ℃, preserving heat for 4-6 hours, and respectively introducing natural gas serving as carbon source gas into two height positions of the first material columns, wherein the ventilation volume of the single first material column is 17m 3 /h-23m 3 Controlling the primary deposition pressure to be 12kPa-15kPa, and controlling the primary deposition time to be 80-100 hours;
preparing a second material column: stopping ventilation and heating after the primary deposition step is finished, cooling the thermal field area through a cooling system, taking out a plurality of prefabricated products generated in the first material column, arranging the prefabricated products in descending order of density in the height direction in sequence, and sleeving a crucible side or an outer guide cylinder outside the prefabricated products to manufacture a second material column;
secondary deposition: setting up a plurality of second material columns in the thermal field area, regulating the pressure in the furnace to be not more than 300Pa, heating the bottom of the thermal field area to 1120-1125 ℃, heating the middle part to 1115-1120 ℃, heating the upper part to 1100-1115 ℃, preserving heat for 4-6 hours, and respectively introducing the carbon source gas into two height positions of the second material columns, wherein the ventilation volume of the single second material column is 14m 3 /h-20m 3 Controlling the secondary deposition pressure to be 8kPa-10kPa, and controlling the secondary deposition time to be 100-120 hours;
processing a semi-finished product: stopping ventilation and heating after the secondary deposition step is finished, cooling the thermal field area, taking out a plurality of semi-finished products generated in the second material column, performing heat treatment on the semi-finished products in an environment of 1600-1900 ℃, and then machining the semi-finished products to a preset size;
preparing a third material column: placing the machined semi-finished products in a lamination manner, sleeving a crucible side or an outer guide cylinder outside the semi-finished products, and sleeving a layer of outer die to manufacture a third material column;
three times of deposition: setting up a plurality of third material columns in a thermal field area in the CVD furnace, and regulating the pressure in the furnaceHeating the bottom of the thermal field region to 1195-1100 ℃, heating the middle to 1085-1190 ℃, heating the upper to 1075-1180 ℃, preserving heat for 4-6 hours, and then respectively introducing the carbon source gas into two height positions of the third material column, wherein the ventilation volume of each third material column is 7m 3 /h-10m 3 And/h, controlling the three-time deposition pressure to be 5kPa-6kPa, and controlling the three-time deposition time to be 40-60 hours, thus obtaining the finished product carbon-carbon thermal field material after the deposition is completed.
Preferably, in the above deposition method, preheating devices corresponding to the number of the material columns are further disposed in the thermal field region, and the first material column, the second material column and the third material column are all disposed above the preheating devices when being built, and the preheating devices are used for preheating the gas entering the material columns.
Preferably, in the above deposition method, in one deposition step, the carbon source gas is introduced into a bottom position and an intermediate height position of the first column, respectively, and a ventilation flow rate ratio of the bottom position and the intermediate height position is 2:1.
Preferably, in the above-described deposition method, in the step of preparing the second stub bar, a plurality of the preforms are stacked in the height direction in front-back.
Preferably, in the above deposition method, in the first deposition step, the first column is a structure with a 36-inch side sleeve and a 33-inch side sleeve, and a carbon fiber preform is arranged inside, or a structure with a 36-inch side sleeve and a 36-inch outer guide cylinder and a carbon fiber preform is arranged inside.
Preferably, in the above deposition method, the first material column is composed of two half material columns which are divided in half vertically, when a single first material column is built, the two half material columns are hoisted and placed in the thermal field region by a hoisting tool in two times, and the structures of the second material column and the third material column are the same as those of the first material column.
Preferably, in the deposition method, the cooling system is a two-stage cooling device, and the first-stage cooling device is a nitrogen pipeline arranged on the side wall of the furnace body, and the flow rate of the nitrogen pipeline is 10m 3 /h-15m 3 Nitrogen gas for/hThe second-stage cooling device is a fast air cooler, and the second-stage cooling device cools the furnace to 900 ℃ through forced air cooling circulation.
Preferably, in the above deposition method, a single said first pillar produces 6-8 said preforms.
Preferably, in the above deposition method, the material of the preheating device is a carbon-carbon composite material.
Preferably, in the above deposition method, in the step of preparing the third material column, the outer mold is a heat-preserving cylinder preform, a heat-preserving cylinder semi-finished product or a carbon-carbon cylinder.
A deposition apparatus for carbon-carbon thermal field material, suitable for performing deposition preparation of carbon-carbon thermal field material by using the deposition method provided in any of the above embodiments, the deposition apparatus comprising:
the thermal field device is used for providing a thermal field environment required by a carbon-carbon thermal field material deposition process, and is provided with three-stage independently-adjusted heating devices along the height direction of the thermal field device, wherein the heating devices comprise a lower zone furnace bottom heater, a middle zone furnace body heating electrode and an upper zone furnace body heating electrode;
the preheating devices are arranged in the thermal field device and are used for bearing a material column arranged in the thermal field device and preheating carbon source gas entering the material column to a temperature range required by cracking of the carbon source gas;
The air inlet device comprises a plurality of pairs of air inlet pipes and air supplementing pipes, wherein the air inlet pipes are arranged in pairs, the air inlet pipes are used for introducing carbon source gas to the bottoms of the material columns, and the air supplementing pipes are used for introducing the carbon source gas to the middle height area of the material columns.
Preferably, in the above deposition apparatus, the deposition apparatus further includes a furnace cover device disposed on top of the thermal field device, the furnace cover device includes a gas collecting hood, the gas collecting hood is configured to collect and guide the gas exhausted from the thermal field device, and the gas collecting hood is provided with a gas outlet on a line where an axis of any one of the material columns is located.
Preferably, in the above deposition apparatus, the deposition apparatus further includes an exhaust gas treatment device in communication with an exhaust end of the gas collection hood, the exhaust gas treatment device including:
the cooling device comprises two groups of gas condensers which are arranged in series and are used for cooling the tail gas and condensing tar in the tail gas;
the dust removing device comprises a cloth bag dust remover for filtering carbon powder, wherein a plurality of small dust removing cloth bags filled with activated carbon are arranged in an array in the cloth bag dust remover;
and the vacuum pump set is arranged at the downstream of the dust removing device and is used for driving tail gas of the thermal field device to flow through the cooling device and the dust removing device.
Preferably, in the above deposition apparatus, the gas condensers are provided with spiral sheets for extending the gas stroke and increasing the heat exchange area, and each of the gas condensers is provided with a receiving chamber at the bottom for storing the condensed tar.
Preferably, in the above deposition apparatus, the exhaust gas treatment device is communicated with the exhaust end of the gas collecting hood through a first pipe, a heat insulation liner is disposed inside the first pipe, and a double-layer water cooling jacket is sleeved outside the first pipe.
Preferably, in the above deposition apparatus, the preheating means includes:
the first preheating plates and the second preheating plates with the same size are alternately stacked and arranged at intervals, the first preheating plates comprise a first annular area, the second preheating plates comprise a second annular area, a plurality of vent holes are formed in the first annular area and the second annular area, the vent holes are used for inputting the carbon source gas through the air inlet pipe, and the small circular radius of the first annular area is larger than the large circular radius of the second annular area;
the first end of the preheating pipeline is communicated with the air supplementing pipe, the second end of the preheating pipeline extends out of a plurality of layers of the first preheating plate and the second preheating plate so as to transmit the carbon source gas in the air supplementing pipe and seal through holes formed in the first preheating plate and the second preheating plate when the carbon source gas passes through the first preheating plate and the second preheating plate;
An outer seal ring provided between any pair of adjacent first and second preheating plates for sealing a space between the adjacent first and second preheating plates at an outer circumferential position of the first preheating plate;
the furnace bottom plate is used for bearing the first preheating plate and the second preheating plate, a middle hole and a peripheral hole are formed in the furnace bottom plate, the middle hole is used for being communicated with the air supplementing pipe and the preheating pipeline, and the peripheral hole is used for being communicated with the air inlet pipe and the vent hole.
Preferably, in the above deposition apparatus, the preheating pipeline includes a first preheating pipeline and a second preheating pipeline that are inserted, the first preheating pipeline is used for butt-jointing a gas channel in the material column, the second preheating pipeline is provided with a protruding portion, and the protruding portion is inserted into a gap between adjacent first preheating plate and second preheating plate and supports the first preheating plate or the second preheating plate.
Preferably, in the above deposition apparatus, a circular ring-shaped air guide ring with a circumferential opening is further provided between adjacent first and second preheating plates, and the air guide ring is used for reducing the passage area of the gas and supporting adjacent first and second preheating plates.
Preferably, in the above deposition apparatus, the materials of the first preheating plate, the second preheating plate and the outer sealing ring are all carbon-carbon composite materials.
Preferably, in the above deposition apparatus, the flow rates of the intake pipe and the air supply pipe are controlled by a mass flow meter, and the flow rate ratio of the intake pipe and the air supply pipe is 2:1.
Preferably, in the above deposition apparatus, the first stub bar includes:
the material column chassis is provided with through holes in the central area and the edge area respectively so as to control the gas in the gas inlet pipe to enter the edge area, and the gas in the gas supplementing pipe enters the central area;
the air inlet of the inner pipe is communicated with a through hole formed in the central area of the material column chassis, and the air outlet is arranged at the middle height position of the first material column;
the carbon fiber prefabricated body is arranged in a layered and independent mode and stacked in the front-back mode;
36 inch crucible side and 33 inch crucible side, 33 inch crucible side cover is located the carbon fiber perform outside, 36 inch crucible side cover is located 33 inch crucible side outside.
Preferably, in the above deposition apparatus, the gas outlet of the inner tube is provided with a gas outlet pipe head, and the gas outlet pipe head is a coaxial cylinder and is uniformly provided with a plurality of gas outlet holes in a circumferential direction, so as to disperse the gas introduced into the inner tube along the circumferential direction of the inner tube.
Preferably, in the above deposition apparatus, a bottom portion of any one of the material columns is provided with one of the lower zone floor heaters, and the lower zone floor heater is surrounded by a heat-retaining member.
Preferably, in the above deposition apparatus, furnace body insulation cotton is laid around the thermal field device, and the insulation cotton is aluminum silicate insulation cotton brick.
Preferably, in the above deposition apparatus, a circumferential integral carbon Ma Futi is provided around the thermal field device, and the circumferential integral carbon Ma Futi is combined with a graphite plate provided at the bottom of the thermal field device to physically seal the thermal field device.
According to the technical scheme, the deposition method of the carbon-carbon thermal field material comprises a primary deposition step, a second material column preparation step, a secondary deposition step, a semi-finished product processing step, a third material column preparation step and a third deposition step, wherein the primary deposition step comprises the steps of constructing a plurality of first material columns in a thermal field area in a CVD furnace, regulating the pressure in the furnace to be not more than 300Pa, heating the bottom of the thermal field area to 1145-1150 ℃ through a three-stage independent heating system arranged along the height direction of the thermal field area, heating the middle part to 1135-1140 ℃, heating the upper part to 1125-1130 ℃, and respectively introducing natural gas serving as carbon source gas into two height positions of the first material columns after heat preservation for 4-6 hours, wherein the ventilation volume of a single first material column is 17m 3 /h-23m 3 /h，The primary deposition pressure is controlled to be 12kPa-15kPa, the primary deposition time is 80h-100h, and the purpose of the primary deposition step is to use a large amount of graphite or carbon-carbon tooling to reduce the density (0.45 g/cm 3 ) As a raw material, by rapid deposition for a short time (80 h-100 h) to obtain a low density (0.8 g/cm) 3 -1.2g/cm 3 ) A carbon-carbon thermal field material preform of (2) is used as a raw material for subsequent deposition; after the prefabricated product is discharged from the furnace, vertically arranging the prefabricated product, sleeving a crucible side or an outer guide cylinder outside the prefabricated product to prepare a second material column, taking the second material column as a production tool to carry out a secondary deposition step, wherein the secondary deposition step is specifically to construct a plurality of second material columns in a thermal field area, adjust the pressure in the furnace to be not more than 300Pa, heat the bottom of the thermal field area to 1120-1125 ℃, heat the middle part to 1115-1120 ℃, heat the upper part to 1100-1115 ℃ and keep the temperature for 4-6 hours, respectively introducing the carbon source gas into two height positions of the second material column, wherein the ventilation volume of each second material column is 14m 3 /h-20m 3 Controlling the secondary deposition pressure to 8kPa-10kPa and the secondary deposition time to 100h-120h, the purpose of the secondary deposition step being to densify the preform by passing a large amount of the carbon source gas through the interlayer, i.e., through the surface of the preform, through the second column bilayer structure, and controlling deposition process parameters (temperature, pressure, natural gas flow and deposition time) to densify the preform to 1.3g/cm 3 -1.5g/cm 3 Obtaining a semi-finished product of the carbon-carbon thermal field material; after finishing the secondary deposition step, carrying out heat treatment and machining on the obtained semi-finished product to obtain a semi-finished product with preset size, stacking and placing the machined semi-finished product, externally sleeving a crucible side or an external guide cylinder, sleeving a layer of outer die to manufacture a third material column, taking the third material column as a production tool to carry out the tertiary deposition step, specifically, setting up a plurality of third material columns in a hot field area in a CVD furnace, regulating the pressure in the furnace to be not more than 300Pa, heating the bottom of the hot field area to 1195-1100 ℃, heating the middle part to 1085-1190 ℃, heating the upper part to 1075-1180 ℃, and preserving heat for 4-6 h, and then, guiding the material column to the CVD furnaceThe carbon source gas is respectively introduced into the two height positions of the third material column, and the ventilation volume of the single third material column is 7m 3 /h-10m 3 Controlling the three-time deposition pressure to be 5kPa-6kPa, the three-time deposition time to be 40h-60h, and obtaining the finished product carbon-carbon thermal field material after the deposition, wherein the three-time deposition step aims to uniformly coat the carbon source gas on the inner and outer surfaces of the semi-finished product so as to further densify the semi-finished product to a density of 1.4g/cm 3 -1.6g/cm 3 And (3) obtaining a carbon-carbon thermal field material with the density meeting the requirement, and forming compact pyrolytic carbon coatings on the inner and outer surfaces of the semi-finished product at the same time so as to improve the silicon vapor corrosion and oxidation resistance of the finished product.
The method for depositing the carbon-carbon thermal field material provided by the invention comprises the steps of carrying out three times of deposition, controlling the technological parameters in the three times of deposition to carry out rapid pre-deposition on the carbon fiber preform, carrying out small molecule densification deposition to improve the density of the product, and finally forming a dense pyrolytic carbon coating on the inner and outer surfaces of the product to improve the service life of the product while further increasing the density by further densification deposition, wherein the different material columns are respectively used in each process to realize the purpose of deposition, the total time of the process is reduced to 240-300 h compared with the prior art by the progressive deposition method, and the density of the obtained finished carbon-carbon thermal field material is 1.4g/cm 3 -1.6g/cm 3 And the qualification rate of the finished product is high.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of a deposition method of a carbon-carbon thermal field material according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a deposition apparatus for carbon-carbon thermal field materials according to an embodiment of the present invention;
FIG. 3 is a schematic view of a thermal field device according to an embodiment of the present invention;
fig. 4 is a schematic structural diagram of an exhaust gas treatment device according to an embodiment of the present invention;
FIG. 5 is a top view of FIG. 2;
FIG. 6 is a schematic diagram of a preheating device according to an embodiment of the present invention;
FIG. 7 is a schematic view of a first preheat plate structure;
FIG. 8 is a schematic view of a second preheat plate structure;
FIG. 9 is a schematic diagram of a first preheating pipeline;
FIG. 10 is a schematic diagram of a second preheating pipeline;
FIG. 11 is a schematic view of an outer seal ring structure;
FIG. 12 is a schematic view of a gas ring structure;
FIG. 13 is a schematic view of the structure of a furnace bottom plate;
FIG. 14 is a schematic view of a first column structure according to an embodiment of the present invention;
FIG. 15 is a schematic view of a column chassis structure;
FIG. 16 is a schematic view of the outlet pipe head;
wherein 1 is a thermal field device, 10 is furnace body heat preservation cotton, 11 is circumferential integral carbon Ma Futi, 12 is graphite plate, 2 is a heating device, 20 is a lower zone furnace bottom heater, 21 is a middle zone furnace body heating electrode, 22 is an upper zone furnace body heating electrode, 3 is a preheating device, 30 is a first preheating plate, 301 is a first annular zone, 3011 is a vent hole, 31 is a second preheating plate, 311 is a second annular zone, 32 is a preheating pipeline, 321 is a first preheating pipeline, 322 is a second preheating pipeline, 3221 is a protruding part, 33 is an outer sealing ring, 34 is a furnace bottom plate, 341 is a middle hole, 342 is a peripheral hole, 35 is an air guide ring, 4 is an air inlet device, 41 is an air inlet pipe, 42 is an air supplementing pipe, 5 is a furnace cover device, 50 is an air collecting cover, 501 is an air outlet, 6 is an exhaust gas treatment device, 60 is a cooling device, 601 is a gas condenser, 6011 is a spiral sheet, 6012 is a containing cavity, 61 is a dust removing device, 611 is a bag-type dust remover, 6110 is a small-sized dust removing bag, 62 is a vacuum pump set, 7 is a first pipeline, 8 is a first material column, 80 is a material column chassis, 81 is an inner pipe, 811 is an air outlet pipeline head, 8110 is an air outlet hole, 82 is a carbon fiber preform, 83 is a 33-inch crucible side, 84 is a 36-inch crucible side, and 9 is a nitrogen pipeline.
Detailed Description
The core of the invention is to disclose a deposition method of a carbon-carbon thermal field material, so as to reduce the preparation process duration and reduce the unit energy consumption and the equipment depreciation rate while ensuring that the prepared carbon-carbon thermal field material has good mechanical properties.
Another core of the present invention is to provide a deposition apparatus for a carbon-carbon thermal field material suitable for the above deposition method.
In order to better understand the solution of the present invention, the following description of the embodiments of the present invention refers to the accompanying drawings. Furthermore, the embodiments shown below do not limit the summary of the invention described in the claims. The whole contents of the constitution shown in the following examples are not limited to the solution of the invention described in the claims.
As shown in fig. 1, the deposition method of the carbon-carbon thermal field material provided by the embodiment of the invention at least includes the steps of:
s01: primary deposition: setting up a plurality of first material columns in a thermal field area in a CVD furnace, regulating the pressure in the furnace to be not more than 300Pa, heating the bottom of the thermal field area to 1145-1150 ℃ through a three-stage independent heating system arranged along the height direction of the thermal field area, heating the middle part to 1135-1140 ℃ and the upper part to 1125-1130 ℃, preserving heat for 4-6 hours, respectively introducing natural gas serving as carbon source gas into two height positions of the first material columns, wherein the ventilation volume of a single first material column is 17m 3 /h-23m 3 Controlling the primary deposition pressure to be 12kPa-15kPa, and controlling the primary deposition time to be 80-100 hours;
it should be noted that, in the above embodiment, the preparation of the carbon-carbon thermal field material is performed by using natural gas as a carbon source gas, and the cracking temperature range of the natural gas is 1075-1175 ℃, so that the related deposition processes are all performed within the cracking temperature range, and similarly, other carbon source gases, such as propane, propylene, etc., need to be adapted to the corresponding cracking temperature ranges for deposition, which will not be repeated herein.
It should be further noted that the purpose of the one deposition step is to use a large number of graphite or carbon-carbon tools to obtain a low density (0.45 g/cm 3 ) As a raw material, by rapid deposition for a short time (80 h-100 h) to obtain a low density (0.8 g/cm) 3 -1.2g/cm 3 ) In step S01, the heating of the thermal field region is a three-layer layered heating system in the height direction, the three-layer heating system is independently controlled to uniform the temperature of the thermal field region, and the temperature of the bottom region is set higher in consideration of the more serious heat escaping from the bottom region, and meanwhile, the three-layer layered heating system can flexibly adjust the temperature in the thermal field region during the deposition process, such as the bottom temperature is low and the top temperature is high after the heating of the thermal field region, and the temperature of the bottom and middle heaters can be adjusted higher and the temperature of the upper heater can be adjusted lower.
In addition, considering that the natural gas in the first material column is gradually consumed and the concentration is reduced in the process of rising and depositing, the product deposition effect at the upper part of the first material column is poor, so in step S01, the natural gas is introduced into two height positions of the first material column, namely, the natural gas is introduced into the first material column from the bottom, and simultaneously, the natural gas is additionally introduced into the other height position of the first material column, so that the product deposition effect of each region on the first material column is uniform.
S02: preparing a second material column: stopping ventilation and heating after the primary deposition step is finished, cooling the thermal field region through a cooling system, taking out a plurality of prefabricated products generated in the first material column, arranging the prefabricated products in descending order of density in the height direction in sequence, and sleeving a crucible side or an outer guide cylinder outside the prefabricated products to manufacture a second material column;
in step S02, after the preforms produced in the first column are taken out, the positions of the preforms are changed in the height direction, that is, the low-density preforms are placed on the upper layer, and the high-density products are placed on the lower layer, so that the density of the products tends to be uniform in the subsequent deposition process.
It should be further noted that the second column is provided with a side wall or an outer guide tube outside the preform to form a gas flow passage for limiting the gas inside and outside, so that the natural gas can flow in full contact with the preform without flowing in the cavity of the preform.
S03: secondary deposition: setting up a plurality of second material columns in the thermal field area, regulating the pressure in the furnace to be not more than 300Pa, heating the bottom of the thermal field area to 1120-1125 ℃, heating the middle part to 1115-1120 ℃, heating the upper part to 1100-1115 ℃, preserving the heat for 4-6 hours, and respectively introducing carbon source gas into two height positions of the second material columns, wherein the ventilation capacity of each second material column is 14m 3 /h-20m 3 Controlling the secondary deposition pressure to be 8kPa-10kPa, and controlling the secondary deposition time to be 100-120 hours;
the purpose of the secondary deposition step is to densify the preform by passing a large amount of carbon source gas through the interlayer, i.e., through the surface of the preform, by the double layer structure of the second column, and controlling the deposition process parameters (temperature, pressure, natural gas flow and deposition time) to densify the preform to 1.3g/cm 3 -1.5g/cm 3 Obtaining a semi-finished product of the carbon-carbon thermal field material;
s04: processing a semi-finished product: stopping ventilation and heating after the secondary deposition step is finished, taking out a plurality of semi-finished products generated in the second material column after the thermal field area is cooled, carrying out heat treatment on the semi-finished products in an environment of 1600-1900 ℃, and then machining the semi-finished products to a preset size;
s05: preparing a third material column: stacking the machined semi-finished products, sleeving a crucible side or an outer guide cylinder outside the semi-finished products, and sleeving a layer of outer die to manufacture a third material column;
S06: three times of deposition: setting up a plurality of third material columns in a thermal field area in a CVD furnace, regulating the pressure in the furnace to be not more than 300Pa, heating the bottom of the thermal field area to 1195-1100 ℃, heating the middle part to 1085-1190 ℃, heating the upper part to 1075-1180 ℃, preserving heat for 4-6 hours, and respectively introducing carbon source gas into two height positions of the third material columns, wherein the ventilation volume of the single third material column is 7m 3 /h-10m 3 Controlling the three-time deposition pressure to be 5kPa-6kPa, and controlling the three-time deposition time to be 40-60 hours, so as to obtain a finished product carbon-carbon thermal field material after the deposition is completed;
the purpose of the three deposition steps is to uniformly coat the inner and outer surfaces of the semi-finished product with the carbon source gas to further densify the semi-finished product to a density of 1.4g/cm 3 -1.6g/cm 3 And (3) obtaining the carbon-carbon thermal field material with the density meeting the requirement, and forming compact pyrolytic carbon coatings on the inner surface and the outer surface of the semi-finished product at the same time so as to improve the silicon vapor corrosion and oxidation resistance of the finished product.
In the above embodiment, in step S01, the carbon fiber preform has a high utilization rate of the carbon source gas, a high deposition densification rate, and a low probability of occurrence of carbon black and encrustation within the initial deposition time of 100 hours. Therefore, the carbon deposition and crusting on the surfaces of the tool and the prefabricated body can be greatly reduced by short-time pre-deposition, so that the workload of cleaning the tool is greatly reduced, and the damage of cleaning the carbon deposition and crusting of the tool is relieved.
In step S03, the second material column is designed to ensure the stability of the air flow field and the pressure field in the material column, and meanwhile, the air flows in the product middle channel arranged in multiple layers, the residence time of the carbon source air is greatly reduced, the deposition is mainly based on deposition of small molecules, the deposition densification in the product is facilitated, the air concentration in the product middle channel is far higher than that in the outer layer product and the inner layer product, the air diffusion power is enhanced, the air diffusion and deposition in the product are facilitated, the air pressure in the product middle channel is higher than that in the outer layer product and the inner layer product, the air forms the pressure forced flow from the middle to the two sides, and the air diffusion to the product is enhanced and the densification is rapidly deposited.
In step S06, the flowing area of the reaction gas is limited in the narrow space between the inner die and the outer die of the third material column, so that the reaction volume of the gas is greatly reduced, the gas residence time is shortened under the same gas inlet flow rate, the concentration of the micromolecular reaction gas in the reaction gas is increased, the gas can continuously permeate into the product to carry out deposition densification so as to increase the density of the product, meanwhile, the high-temperature and high-pressure process parameters are adopted to greatly improve the deposition speed, and after the inside of the product is rapidly densified, the surface of the product rapidly forms a dense pyrolytic carbon coating so as to improve the silicon vapor corrosion and oxidation resistance, thereby prolonging the service life of the thermal field material.
The carbon-carbon thermal field material deposition method provided by the embodiment of the invention comprises the steps of carrying out three deposition steps in total, and controlling the technological parameters in the three deposition steps to carry out rapid pre-deposition on the carbon fiber preform, then carrying out small molecule densification deposition to improve the product density, and finally forming a dense pyrolytic carbon coating on the inner and outer surfaces of the product to improve the service life and mechanical properties of the product while further increasing the density by further densification deposition, wherein the different material columns with different structures are respectively used in each process to achieve the corresponding deposition purpose, the total process duration is obviously reduced by the progressive deposition method, namely the process duration of 600-700 h is reduced to 240-300 h from that of 600.4 g/cm in the prior art, and the density of the obtained finished carbon-carbon thermal field material is 1.4g/cm 3 -1.6g/cm 3 In a specific embodiment of the invention, seven material columns are arranged in the hot field area at a time, and each material column is used for producing eight products, wherein each layer of products are charged in layers independently, so that the products between the layers do not generate interaction force, the risk of bearing deformation of the products is eliminated, and the unit energy consumption and the equipment depreciation rate are reduced by improving the single yield.
In addition, the method and the apparatus for controlling the pressure in the thermal field area are the same as those in the prior art, and are not described herein.
Further, in order to avoid a great amount of cold air continuously entering the bottom of the material column to cause the temperature of the material column to decrease when the carbon source gas is input into the material column, in a specific embodiment of the present invention, a preheating device is further disposed in the hot field area, the number of the preheating device is not less than the number of the material columns in a single deposition process, and the first material column, the second material column and the third material column are all disposed above the preheating device when being set up, and the preheating device is used for preheating the gas entering the material column.
In one embodiment of the present invention, the preheating device is a gas flow channel which is spirally arranged, and the purpose of preheating gas is achieved by prolonging the gas flow stroke.
Further, in order to further enhance the uniformity of the density of the product during the deposition process, in an embodiment of the present invention, the natural gas is introduced into two height positions of the first material column, wherein the two height positions are a bottom position and a middle height position of the material column, respectively, and the ventilation flow ratio of the bottom position and the middle height position is 2:1.
Further, in one embodiment of the present invention, when the second material column is prepared, a plurality of prefabricated products are stacked in the height direction, so as to form a gas channel with streamline shape, reduce turbulence formed at dead angles in the gas flow process, reduce the extension of gas residence time caused by gas turbulence, and further avoid the generation of macromolecular or even carbon black and other substances on the surface of the product due to gas phase nucleation generated by long-time residence of gas.
Further, in a specific embodiment of the present invention, in step S01, the first material column is a 36-inch crucible side sleeve 33-inch crucible side, and a carbon fiber preform structure is provided in the first material column to correspondingly perform preparation of the crucible side, and the first material column may also be a 36-inch crucible side sleeve 36-inch outer guide cylinder and a carbon fiber preform structure is provided in the first material column to correspondingly perform preparation of the guide cylinder.
Further, the first material column is composed of two half material columns which are vertically and semi-separated, so that the loading of each layer of products in the first material column is facilitated, meanwhile, when a single first material column is built, the two half material columns are hoisted and placed in a thermal field area for splicing through a lifting appliance twice, and the pressure in the thermal field area is pumped to below 300Pa by a vacuum pump.
The structures of the second material column and the third material column and the hoisting method in the hot field area are the same as those of the first material column.
Further, in order to accelerate the cooling of the thermal field region and the material column after the single deposition step is completed and further shorten the total process time, in an embodiment of the present invention, the cooling system for cooling the thermal field region is a two-stage cooling device, wherein the first-stage cooling device is a nitrogen pipeline or a nitrogen pipeline arranged on the sidewall of the furnace body A rapid cooling air inlet pipeline arranged at the furnace bottom, and after ventilation and heating of a thermal field area are stopped, the continuous flow rate of 10m after micro positive pressure in the furnace is maintained 3 /h-15m 3 Cooling with nitrogen gas of/h; the second-stage cooling device is a fast air cooler, which cools down through forced air cooling circulation after the temperature in the furnace is reduced to 900 ℃, and can close the cooling system after cooling to 200 ℃, and the furnace is opened to take out the product.
Further, in the deposition method provided by the embodiment of the invention, 6-8 preforms are produced by a single first material column, wherein the preforms are vertically arranged in a single layer, a partition plate is arranged between two adjacent layers to avoid stress deformation of the adjacent preforms, and the purpose of producing multi-layer products in the single material column is ensured by a three-stage independent heating system in the height direction and two high ventilation systems, and preferably, the production of 8 preforms is carried out by the single first material column.
It should be noted that, in the single carbon-carbon thermal field material production process, the second material column and the third material column are the same as the first material column in structure and product production quantity.
Further, in step S05, the outer mold is a heat-insulating cylinder preform, a heat-insulating cylinder semi-finished product, or a carbon-carbon cylinder.
As shown in fig. 2, the embodiment of the present invention further provides a deposition apparatus for a carbon-carbon thermal field material, which is suitable for performing deposition preparation of the carbon-carbon thermal field material by using the deposition method provided in any one of the embodiments, specifically, as shown in fig. 3, fig. 4 and fig. 5, the deposition apparatus includes a thermal field device 1, a preheating device 3 and an air intake device 4, so that the thermal field is adapted to each deposition process in the deposition method provided in the embodiment, where the thermal field device 1 is used for providing a thermal field environment required by the deposition process of the carbon-carbon thermal field material, and it is to be noted that the thermal field device 1 is an existing device for providing a thermal field region in a CVD furnace, and in particular, the thermal field device 1 provided in the embodiment of the present invention is provided with a three-stage independently regulated heating device 2 along a height direction thereof, the heating device 2 includes a lower zone hearth heater 20, a middle zone hearth heater electrode 21 and an upper zone hearth heater electrode 22, where the lower zone hearth heater 20 is used for heating a bottom of the thermal field device 1, preferably the lower zone hearth heater 20 is a heater and the carbon heater is an integral heater of the thermal field device 1, and the thermal field device 1 is used for reducing a thermal field failure rate of the composite heater, and reducing a service life of the heater; the middle zone furnace body heating electrode 21 is a heating electrode which surrounds the thermal field device 1 from the bottom to the middle height of the thermal field device 1, the upper zone furnace body heating electrode 22 is a heating electrode which surrounds the thermal field device 1 from the middle height to the top of the thermal field device 1, and the three zones of the heating device 2 which are independently controlled and regulated can independently set control temperature points of each zone according to the charging characteristics, the temperature field distribution after full load and CVI process ventilation, so as to achieve the purpose of uniform furnace temperature field.
It should be noted that, in order to prevent the heater of each partition from being pyrolyzed by deposition in the deposition atmosphere, especially at the position of the heater electrode, so that all three heating areas are sealed by physical isolation from the deposition area, in one embodiment of the present invention, the furnace body is physically sealed by using upper and lower spliced circumferential integral carbon Ma Futi 11, and at the same time, the sealed heating areas are filled with nitrogen gas to make the pressure higher than that of the deposition area, so as to protect the electrode from being shorted by deposition or being ignited.
It should be further noted that, in the above embodiment, the heating device 2 is arranged in three layers along the height of the thermal field device 1, it is easy to think that more layers of individually controlled heating devices 2 can be arranged along the height direction of the thermal field device 1, so as to improve the uniformity of the thermal field in the furnace, and the technical solution of individually adjusting more layers of the heating device 2 is also within the scope of the present invention.
In addition, the heating device 2 needs to be cooled after the single deposition process is completed, wherein the first stage of cooling is performed by introducing nitrogen into a nitrogen pipeline 9 arranged on the side wall of the heating device 2 for cooling, and the flow of the introduced nitrogen is preferably 10m 3 /h-15m 3 /h。
On the other hand, the preheating device 3 is provided with a plurality of preheating devices 3 for carrying each material column placed in the thermal field, so that the number of the preheating devices 3 in the thermal field device 1 is not less than the number of the material columns, the preheating devices 3 are used for preheating the carbon source gas to be introduced into the material columns to a temperature range required by cracking the carbon source gas, so that the carbon source gas can be deposited when entering the material columns, the deposition effect of the product at the bottom of the material columns is poor due to the fact that the gas is not cracked at the bottom of the material columns, and meanwhile, the problem that the deposition density of the product is too low due to the fact that the temperature of the main bottom of the material columns is reduced due to the fact that a large amount of cold gas enters can be avoided.
And for the air inlet device 4 in the deposition equipment, the air inlet device comprises an air inlet pipe 41 and an air supplementing pipe 42 which are arranged in pairs, the air inlet pipe 41 and the air supplementing pipe 42 are used for conveying carbon source gas to a single material column, specifically, the air inlet pipe 41 is communicated with the bottom of the material column so as to input the carbon source gas to the bottom of the material column, and as the carbon source gas is gradually consumed in the process of rising along the material column and the concentration is reduced, the deposition effect of the upper-layer product of the material column is poor, the air supplementing pipe 42 is arranged, and one end of the air supplementing pipe 42 extends into the middle height area of the material column so as to supplement air to the middle height area of the material column.
It should be noted that, a pipeline which is directly connected to the middle of the material column is preferably disposed in the material column tooling, so as to supply air to the air supplementing pipe 42.
According to the deposition equipment provided by the embodiment of the invention, a thermal field device 1 is used for providing a thermal field environment required by a deposition process, and particularly, a heating device 2 which is independently regulated in three stages is arranged in a thermal field area along the height direction, so that the temperature uniformity of the thermal field environment is ensured through regional temperature control, meanwhile, a plurality of preheating devices 3 are arranged in the thermal field device 1 to preset the inlet air of a material column, the cracking state of carbon source gas is ensured when the carbon source gas enters the bottom of the material column, the qualification rate of products produced at the bottom of the material column is improved, and in addition, in order to improve the uniformity and consistency of the products in the material column, an air inlet device 4 is used for respectively supplying air at the bottom and middle height area of each material column, so that the density of the carbon source gas at the upper part and the lower part in the material column is uniform, and the deposition effect of each material column is ensured.
Further, in an embodiment of the present invention, the deposition apparatus further includes a furnace cover device 5 disposed at the top of the thermal field device 1, the furnace cover device 5 is used for insulating and sealing the thermal field device 1, meanwhile, the furnace cover device 5 includes a gas collecting cover 50, the gas collecting cover 50 is used for collecting and guiding the gas discharged during the deposition process of the material column in the thermal field device 1, that is, a plurality of gas outlets 501 are formed on the gas collecting cover 50 to discharge the gas in the thermal field device 1, and since the gas in the material column flows along the direction of the material column, it is preferable that the gas outlet 501 is disposed on the line where the axis of any material column is located in the gas collecting cover 50, that is, after the gas is discharged from the top of the material column, the gas continues to flow upward along the vertical direction and is discharged from the gas outlet 501 of the gas collecting cover 50.
Further, on the basis of the above embodiment, as shown in fig. 2 and fig. 4, the exhaust end of the gas collecting hood 50 is communicated with the exhaust gas treatment device 6 to cool and filter the exhaust gas generated in the thermal field device 1, so as to avoid the exhaust gas from polluting the environment greatly, specifically, the exhaust gas treatment device 6 includes a cooling device 60, a dust removal device 61 and a vacuum pump set 62, wherein the cooling device 60 includes a gas condenser 601 for cooling the exhaust gas, especially for cooling tar in the exhaust gas, and the gas condensers 601 are preferably arranged in series to form two groups, so as to avoid the overload of a single gas condenser 601 and to be standby; the dust removing device 61 is generally disposed downstream of the cooling device 60 to filter carbon powder in the tail gas, in a preferred embodiment of the present invention, the dust removing device 61 includes a bag-type dust remover 611, and a plurality of small dust removing bags 6110 with activated carbon inside are disposed in an array inside the bag-type dust remover 611, so as to increase the contact area between the dust removing device 61 and the tail gas, and improve the filtering effect; the vacuum pump set 62 is arranged at the downstream of the dust removing device 61, is used for driving the tail gas of the thermal field device 1 to flow through the cooling device 60 and the dust removing device 61, and is arranged at the downstream of the dust removing device 61, so that impurities entering the vacuum pump set 62 can be reduced, and the service life of the vacuum pump set 62 can be prolonged.
In order to further optimize the above technical solution, on the basis of the above embodiment, the gas condenser 601 is internally provided with the spiral sheet 6011, the spiral sheet 6011 is spirally arranged along the axial direction of the gas condenser 601 to prolong the travel of tail gas in the gas condenser 601, so that the heat exchange time of the tail gas in the gas condenser 601 is prolonged, the heat exchange effect is improved, and the bottom of each gas condenser 601 is provided with the accommodating cavity 6012 for storing condensed tar, so as to store cooled tar, the accommodating cavity 6012 can be provided with a material outlet for discharging tar, and can also be spirally connected with the main body of the gas condenser 601 so as to screw down for discharging tar when a sufficient amount of tar is contained.
Further, in an embodiment of the present invention, the exhaust gas treatment device 6 is communicated with the exhaust end of the gas collecting hood 50 through the first pipe 7, and the first pipe 7 is used as a channel through which the exhaust gas passes first after being discharged, an insulation lining is arranged inside the first pipe to prevent the metal pipe wall from being too high in temperature, and meanwhile, a double-layer water cooling pipe is nested outside the first pipe 7 to primarily cool the exhaust gas passing through the first pipe 7.
In a specific embodiment of the present invention, the preheating device 3 achieves preheating of the gas by extending the stroke of the gas so that the gas obtains more heating time, and in particular, as shown in fig. 6, the preheating device 3 includes a first preheating plate 30, a second preheating plate 31, a preheating pipe 32, an outer sealing ring 33, and a furnace bottom plate 34, wherein, as shown in fig. 7 to 13, the first preheating plate 30 and the second preheating plate 31 are the same in size so that the first preheating plate 30 and the second preheating plate 31 can be regularly stacked, the first preheating plate 30 and the second preheating plate 31 are each plural and are alternately stacked, spaced to form any adjacent two plates as the first preheating plate 30 and the second preheating plate 31, and a spacing interlayer is used for passing the carbon source gas, in particular, the first preheating plate 30 includes a first annular region 301 concentric therewith, the second preheating plate 31 includes a second annular region 311 concentric therewith, the first annular region 301 and the second annular region 311 are each provided with a plurality of ventilation holes 3011, the ventilation holes 3011 are used for carbon source gas input through the air inlet pipe 41, and the small radius of the first annular region 301 is larger than the large radius of the second annular region 311, so that when the side circumferences of the multi-layered first preheating plate 30 and the second preheating plate 31 are sealed, the carbon source gas input from the bottom sequentially passes along the ventilation holes 3011 on each layer of preheating plate, and flows in an S shape in cross section due to the sizes of the first annular region 301 and the second annular region 311, thereby achieving the purpose of prolonging the gas flow stroke.
Meanwhile, considering that the gas delivery height in the gas supplementing pipe 42 is high, the stroke thereof meets the preheating requirement, and in order to ensure timely delivery of the gas in the gas supplementing pipe 42, in the preheating device 3, the first end of the preheating pipeline 32 is communicated with the gas supplementing pipe 42, the second end extends out of the plurality of layers of the first preheating plate 30 and the second preheating plate 31, so that when the carbon source gas in the gas supplementing pipe 42 is delivered and passes through the first preheating plate 30 and the second preheating plate 31 in a sealing manner, through holes are formed in the first preheating plate 30 and the second preheating plate 31, the preheating pipeline 32 passes through the first preheating plate 30 and the second preheating plate 31 which are arranged in a plurality of layers, so that the gas in the gas supplementing pipe 42 passes through the first preheating plate 30 and the second preheating plate 31 to be directly delivered, and is preheated in the delivery process, and meanwhile, the circumference of the gas supplementing pipe 42 and the first preheating plate 30 and the second preheating plate 31 are sealed for smooth preheating of the gas in the gas inlet pipe 41, so that gas leakage in the gas inlet pipe 41 is avoided.
In order to ensure the tightness of the side circumferences of the first preheating plate 30 and the second preheating plate 31, an outer sealing ring 33 is provided between any pair of adjacent first preheating plates 30 and second preheating plates 31, the outer sealing ring 33 seals the interval between the adjacent first preheating plates 30 and second preheating plates 31 from the outer circumferential position, and ensures the stability of the interval between the adjacent first preheating plates 30 and second preheating plates 31, ensuring the structure of the gas flow passage.
In addition, the above structures are all arranged on the furnace bottom plate 34 and carried by the furnace bottom plate 34, and the furnace bottom plate 34 is provided with a middle hole 341 and a peripheral hole 342, wherein the middle hole 341 is used for communicating the air supplementing pipe 42 and the preheating pipeline 32, and the peripheral hole 342 is used for communicating the air inlet pipe 41 and the air vent 3011, so that the carbon source gas in the air supplementing pipe 42 and the air inlet pipe 41 is smoothly split.
In order to further optimize the above technical solution, in a specific embodiment of the present invention, the preheating pipeline 32 includes a first preheating pipeline 321 and a second preheating pipeline 322 that are inserted, where the second preheating pipeline 322 is provided with a plurality of second preheating pipelines 322, the plurality of second preheating pipelines 322 are inserted and arranged to form a main body of the preheating pipeline 32, and the single second preheating pipeline 322 is provided with a protrusion 3221, where the protrusion 3221 is used to be inserted into a gap between the adjacent first preheating plate 30 and second preheating plate 31, so as to effectively seal the gap between the adjacent first preheating plate 30 and second preheating plate 31, and support the first preheating plate 30 or the second preheating plate 31, and the first preheating pipeline 321 is used to interface a gas channel in a material column, that is, the first preheating pipeline 321 is inserted and arranged at one end of the plurality of second preheating pipelines 322, so as to realize the delivery of the carbon source gas.
In order to further optimize the above technical solution, an annular air guide ring 35 is further disposed in the interval between the adjacent first preheating plate 30 and second preheating plate 31, two sides of the air guide ring 35 contact the first preheating plate 30 and the second preheating plate 31, and the periphery of the air guide ring 35 is perforated to block the carbon source gas by the air guide ring 35, and the carbon source gas passes through the openings of the periphery of the air guide ring 35, so that the passing area of the gas is reduced to prolong the passing time of the carbon source gas, and further the preheating effect is improved.
Further, the first preheating plate 30, the second preheating plate 31 and the outer sealing ring 33 are all made of carbon-carbon composite materials, so as to reduce the loss caused by cleaning carbon deposition and disassembly.
Further, in an embodiment of the present invention, the flow rates of the air inlet pipe 41 and the air supplementing pipe 42 are accurately controlled by mass flow meters, and the flow rate ratio of the air inlet pipe 41 to the air supplementing pipe 42 is 2:1.
It should be noted that, the height setting of the air compensating pipe 42 and the flow ratio of the air inlet pipe 41 to the air compensating pipe 42 may be adjusted according to the actual working conditions, and the technical scheme of only adjusting the height of the air compensating pipe 42 and the flow ratio of the air inlet pipe 41 to the air compensating pipe 42 is also within the protection scope of the present invention.
Further, in an embodiment of the present invention, a first column 8 is described, as shown in fig. 14, 15 and 16, the first column 8 includes a column bottom plate 80, an inner tube 81, a fiber preform 36 inch crucible side 84 and a 33 inch crucible side 83, wherein the column bottom plate 80 is provided with through holes in a central region and an edge region, respectively, for dividing carbon source gas, specifically for controlling a gas inlet edge region in the gas inlet tube 41, starting from a bottom of the first column 8, flowing upward, controlling a gas inlet center region in the gas supply tube 42 to flow into an intermediate height position of the first column 8, and for controlling a gas passage in the gas supply tube 42, by means of the inner tube 81 provided in the first column 8, a gas inlet of the inner tube 81 is communicated with a through hole provided in the central region of the column bottom plate 80, a gas outlet 501 thereof is provided in an intermediate height position of the first column 8, in order to directly convey the gas in the gas supplementing pipe 42 to the middle height position of the first material column 8, in addition, the multi-layer carbon fiber preform 82 is independently arranged in layers and stacked in opposite directions, so as to obtain a pre-product which is arranged in opposite directions in one deposition process, the opposite directions can form a streamline gas channel, turbulence is formed at dead angles in the gas flowing process, the prolonging effect of the gas turbulence on the gas residence time is reduced, and further, the generation of macromolecular or even carbon black and other substances on the surface of the product due to long-time gas-phase nucleation generated by the gas residence is avoided, in addition, the 33 inch crucible side 83 is sleeved on the outer side of the carbon fiber preform 82, meanwhile, the 36 inch crucible side 84 is sleeved on the outer side of the 33 inch crucible side 83, so as to form a gas flow channel along the outer side of the carbon fiber preform 82, and form the appearance structure of the first material column 8, it is to be noted that, the 33 inch crucible side 83 can also be replaced with an outer cylinder for the production and preparation of the cylinder.
It should be further noted that, the tooling structure of the second material column and the third material column is similar to that of the first material column 8, and the gas is split by the material column chassis 80, and the gas in the gas supplementing pipe 42 is discharged at the middle height of the material column by the inner pipe 81, and the difference is the difference of the internal filling material and the number of layers of the mold, and the difference is already described in the deposition method of the carbon-carbon thermal field material provided by the embodiment of the present invention, and will not be described again.
In order to further optimize the above technical solution, in the first material column 8, the air outlet 501 of the inner tube 81 is provided with an air outlet pipe head 811, the air outlet pipe head 811 is located at the middle height position of the first material column 8, and the air outlet pipe head 811 is of a coaxial cylindrical structure, wherein the first cylinder is used for communicating the air outlet 501 to allow carbon source gas to enter the air outlet pipe head 811, the diameter of the second cylinder is larger than that of the first cylinder, the second cylinder is uniformly provided with a plurality of air outlet holes 8110 in the circumferential direction, and the carbon source gas reaching the air outlet pipe head 811 is discharged from the plurality of air outlet holes 8110, so that the carbon source gas is uniformly dispersed along the circumferential direction of the air outlet pipe head 811, and further the air supplementing effect at the middle height position of the first material column 8 is improved.
Further, in one embodiment of the present invention, a plurality of lower zone hearth heaters 20 are provided, and a lower zone hearth heater 20 is provided at the bottom of any one column to independently heat the bottom of the column, so that the heating effect is better, and a heat insulation component is provided at Zhou Juanwei of the lower zone hearth heater 20 to reduce heat dissipation of the hearth heater when heating the column.
Further, in the deposition apparatus provided by the embodiment of the invention, furnace body insulation cotton 10 is laid around the thermal field device 1, and the insulation cotton is preferably aluminum silicate insulation cotton bricks.
It should be noted that the thermal field device 1 is a sealed thermal field environment, so that it needs to have a good thermal insulation body to ensure the thermal field effect, and has a thermal insulation structure identical to that of the CVD furnace in the prior art, and will not be described in detail herein.
Further, in an embodiment of the present invention, the thermal field device 1 is provided with a circumferential integral carbon Ma Futi around the periphery, and the circumferential integral carbon Ma Futi is combined with the graphite plate 12 disposed at the bottom of the thermal field device 1 to physically seal the thermal field device 1, which improves the heat preservation effect of the thermal field device 1, and can separate the thermal field device 1 and the heating device 2, so as to improve the service life of the heating device 2 and reduce the maintenance damage rate.
The terms "first," "second," "third," "left" and "right" in the description and claims of the invention and in the above-described figures, etc. are used for distinguishing between different objects and not for describing a particular sequential order. Furthermore, the terms "comprise" and "have," as well as any variations thereof, are intended to cover a non-exclusive inclusion. For example, a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to the listed steps or elements but may include steps or elements not expressly listed.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (24)
1. A method for depositing a carbon-carbon thermal field material, comprising at least the steps of:
primary deposition: setting up a plurality of first material columns in a thermal field area in a CVD furnace, regulating the pressure in the furnace to be not more than 300Pa, heating the bottom of the thermal field area to 1145-1150 ℃ by a three-stage independent heating system arranged along the height direction of the thermal field area, heating the middle part to 1135-1140 ℃ and the upper part to 1125-1130 ℃, preserving heat for 4-6 hours, respectively introducing natural gas serving as carbon source gas into two height positions of the first material columns, wherein the ventilation amount of the single first material column is 17m 3 /h-23m 3 Controlling the primary deposition pressure to be 12kPa-15kPa, and controlling the primary deposition time to be 80-100 hours;
preparing a second material column: stopping ventilation and heating after the primary deposition step is finished, cooling the thermal field area through a cooling system, taking out a plurality of prefabricated products generated in the first material column, arranging the prefabricated products in descending order of density in the height direction in sequence, and sleeving a crucible side or an outer guide cylinder outside the prefabricated products to manufacture a second material column;
secondary deposition: setting up a plurality of second material columns in the thermal field area, regulating the pressure in the furnace to be not more than 300Pa, heating the bottom of the thermal field area to 1120-1125 ℃, heating the middle part to 1115-1120 ℃, heating the upper part to 1100-1115 ℃, preserving heat for 4-6 hours, and respectively introducing the carbon source gas into two height positions of the second material columns, wherein the ventilation volume of the single second material column is 14m 3 /h-20m 3 Controlling the secondary deposition pressure to be 8kPa-10kPa, and controlling the secondary deposition time to be 100-120 hours;
processing a semi-finished product: stopping ventilation and heating after the secondary deposition step is finished, cooling the thermal field area, taking out a plurality of semi-finished products generated in the second material column, performing heat treatment on the semi-finished products in an environment of 1600-1900 ℃, and then machining the semi-finished products to a preset size;
Preparing a third material column: placing the machined semi-finished products in a lamination manner, sleeving a crucible side or an outer guide cylinder outside the semi-finished products, and sleeving a layer of outer die to manufacture a third material column;
three times of deposition: setting up a plurality of third material columns in a thermal field area in a CVD furnace, regulating the pressure in the furnace to be not more than 300Pa, heating the bottom of the thermal field area to 1195-1100 ℃, heating the middle part to 1085-1190 ℃, heating the upper part to 1075-1180 ℃, preserving heat for 4-6 hours, and respectively introducing the carbon source gas into two height positions of the third material columns, wherein the ventilation amount of the single third material column is 7m 3 /h-10m 3 Controlling the three-time deposition pressure to be 5kPa-6kPa, and controlling the three-time deposition time to be 40-60 hours, so as to obtain a finished product carbon-carbon thermal field material after the deposition is completed;
the deposition method is realized by a deposition apparatus including:
the thermal field device (1) is used for providing a thermal field environment required by a carbon-carbon thermal field material deposition process, the thermal field device (1) is provided with three-stage independently-adjusted heating devices (2) along the height direction of the thermal field device, the heating devices (2) comprise a lower zone furnace bottom heater (20), a middle zone furnace body heating electrode (21) and an upper zone furnace body heating electrode (22);
The preheating devices (3) are arranged in the thermal field device (1), and the preheating devices (3) are used for bearing a material column arranged in the thermal field device (1) and preheating carbon source gas entering the material column to a temperature range required by cracking;
the air inlet device (4) comprises a plurality of pairs of air inlet pipes (41) and air supplementing pipes (42) which are arranged in pairs, wherein the air inlet pipes (41) are used for introducing carbon source gas to the bottom of the material column, and the air supplementing pipes (42) are used for introducing the carbon source gas to the middle height area of the material column.
2. The deposition method according to claim 1, wherein preheating devices corresponding to the number of the material columns one by one are further provided in the thermal field region, and the first material column, the second material column and the third material column are all disposed above the preheating devices when being built, and the preheating devices are used for preheating the gas entering the material columns.
3. The deposition method according to claim 1, wherein in one deposition step, the carbon source gas is introduced into a bottom position and an intermediate height position of the first column, respectively, and a ventilation flow rate ratio of the bottom position and the intermediate height position is 2:1.
4. The deposition method of claim 1 wherein a plurality of said preforms are stacked in the height direction in the step of preparing the second column.
5. The deposition process of claim 1 wherein in one deposition step, the first column is a 36 inch crucible side 33 inch side, a carbon fiber preform built-in structure, or a 36 inch crucible side 36 inch outer guide shell, a carbon fiber preform built-in structure.
6. The deposition method according to claim 1, wherein the first material column is composed of two half material columns which are divided in half vertically, the two half material columns are hoisted and placed in the thermal field region by a hoist in two times when a single first material column is built, and the structures of the second material column and the third material column are the same as those of the first material column.
7. The deposition method according to claim 1, wherein the cooling system is a two-stage cooling device, and the first-stage cooling device is a nitrogen gas line provided on a side wall of the furnace body at a flow rate of 10m 3 /h-15m 3 And/h, cooling by nitrogen, wherein the second-stage cooling device is a fast air cooler, and cooling by forced air cooling circulation after the temperature in the furnace is reduced to 900 ℃.
8. The deposition method of claim 1 wherein a single said first column produces between 6 and 8 said preforms.
9. The deposition method of claim 2, wherein the preheating device is a carbon-carbon composite.
10. The deposition method of claim 1, wherein in the step of preparing the third stub bar, the outer mold is a thermal cylinder preform, a thermal cylinder half-product, or a carbon-carbon cylinder.
11. The deposition method according to claim 1, wherein the deposition apparatus further comprises a furnace lid device (5) arranged on top of the thermal field device (1), the furnace lid device (5) comprising a gas collecting hood (50), the gas collecting hood (50) being adapted to collect and guide the gas discharged from the thermal field device (1), the gas collecting hood (50) being provided with a gas outlet (501) in a line where the axis of any one of the material columns is located.
12. The deposition method according to claim 11, wherein the deposition apparatus further comprises an exhaust gas treatment device (6) in communication with the exhaust end of the gas collection hood (50), the exhaust gas treatment device (6) comprising:
a cooling device (60) comprising two groups of gas condensers (601) which are arranged in series and are used for cooling the tail gas and condensing tar in the tail gas;
The dust removing device (61) comprises a cloth bag dust remover (611) for filtering carbon powder, wherein a plurality of small dust removing cloth bags (6110) filled with activated carbon are arranged in the cloth bag dust remover (611) in an array manner;
and the vacuum pump set (62) is arranged at the downstream of the dust removing device (61) and is used for driving the tail gas of the thermal field device (1) to flow through the cooling device (60) and the dust removing device (61).
13. The deposition method according to claim 12, wherein the gas condensers (601) are built with spiral sheets (6011) for extending the gas stroke and increasing the heat exchange area, and a receiving chamber (6012) for storing the condensed tar is provided at the bottom of each gas condenser (601).
14. The deposition method according to claim 12, wherein the exhaust gas treatment device (6) is communicated with the exhaust end of the gas collection cover (50) through a first pipeline (7), a heat preservation lining is arranged inside the first pipeline (7), and a double-layer water cooling jacket is sleeved outside the first pipeline.
15. A deposition method according to claim 1, wherein the preheating means (3) comprise:
the device comprises a first preheating plate (30) and a second preheating plate (31) which are the same in size, wherein a plurality of the first preheating plates (30) and the second preheating plates (31) are alternately stacked and arranged at intervals, the first preheating plate (30) comprises a first annular area (301), the second preheating plate (31) comprises a second annular area (311), a plurality of vent holes (3011) are formed in the first annular area (301) and the second annular area (311), the vent holes (3011) are used for the carbon source gas input through the air inlet pipe (41), and the small circular radius of the first annular area (301) is larger than the large circular radius of the second annular area (311);
A preheating pipeline (32), wherein a first end of the preheating pipeline (32) is communicated with the air supplementing pipe (42), and a second end of the preheating pipeline extends out of a plurality of layers of the first preheating plate (30) and the second preheating plate (31) so as to transmit the carbon source gas in the air supplementing pipe (42) and seal through holes formed in the first preheating plate (30) and the second preheating plate (31) when the carbon source gas passes through the first preheating plate (30) and the second preheating plate (31);
an outer seal ring (33) provided between any pair of adjacent first and second preheating plates (30, 31) for sealing a space between the adjacent first and second preheating plates (30, 31) at an outer peripheral position of the first preheating plate (30);
furnace bottom plate (34) is used for bearing first preheating plate (30) with second preheating plate (31), intermediate hole (341) and peripheral hole (342) have been seted up to furnace bottom plate (34), intermediate hole (341) are used for communicating make-up pipe (42) with preheat pipeline (32), peripheral hole (342) are used for communicating intake pipe (41) with air vent (3011).
16. The deposition method according to claim 15, wherein the preheating line (32) comprises a first preheating line (321) and a second preheating line (322) which are inserted, the first preheating line (321) being used for abutting the gas channel in the material column, the second preheating line (322) being provided with a protrusion (3221), the protrusion (3221) being inserted into a gap between adjacent first preheating plates (30) and second preheating plates (31) and supporting the first preheating plates (30) or the second preheating plates (31).
17. A deposition method according to claim 15, wherein a circumferential perforated annular gas ring (35) is further provided between adjacent first (30) and second (31) pre-heating plates, the gas ring (35) being adapted to reduce the passage area of gas and to support adjacent first (30) and second (31) pre-heating plates.
18. The deposition method according to claim 15, wherein the first preheating plate (30), the second preheating plate (31) and the outer sealing ring (33) are all made of carbon-carbon composite materials.
19. The deposition method according to claim 1, wherein the flow rates of the intake pipe (41) and the gas supply pipe (42) are controlled by a mass flow meter, and the flow rate ratio of the intake pipe (41) and the gas supply pipe (42) is 2:1.
20. The deposition method of claim 1, wherein the first stub bar comprises:
a column base plate (80) with through holes respectively arranged in a central area and an edge area for controlling the gas in the gas inlet pipe (41) to enter the edge area, and the gas in the gas supplementing pipe (42) to enter the central area;
the air inlet of the inner pipe (81) is communicated with a through hole formed in the central area of the material column chassis (80), and the air outlet (501) is arranged at the middle height position of the first material column (8);
a carbon fiber preform (82), wherein a plurality of layers of the carbon fiber preform (82) are arranged in a layered and independent manner and stacked in a positive and negative manner;
36 inch crucible side (84) and 33 inch crucible side (83), 33 inch crucible side (83) cover is located carbon fiber perform (82) outside, 36 inch crucible side (84) cover is located 33 inch crucible side (83) outside.
21. The deposition method according to claim 20, wherein the gas outlet (501) of the inner tube (81) is provided with a gas outlet pipe head (811), and the gas outlet pipe head (811) is a coaxial cylinder and is provided with a plurality of gas outlet holes (8110) uniformly in the circumferential direction, for dispersing the gas introduced into the inner tube (81) along the circumferential direction of the inner tube (81).
22. The deposition method according to claim 1, wherein a bottom of any one of the material columns in the deposition apparatus is provided with one of the lower zone floor heaters (20), and the lower zone floor heater (20) is surrounded with a heat-retaining member.
23. The deposition method according to claim 1, characterized in that furnace insulation cotton (10) is laid around the thermal field device (1), and the insulation cotton is aluminum silicate insulation cotton brick.
24. The deposition method according to claim 1, wherein the thermal field device (1) Zhou Juanwei is provided with a circumferential monolithic carbon Ma Futi (11), the circumferential monolithic carbon Ma Futi (11) being combined with a graphite plate (12) arranged at the bottom of the thermal field device (1) to physically seal the thermal field device (1).
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