CN110963815B - Process for preparing large-size carbon/carbon heating body - Google Patents
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/614—Gas infiltration of green bodies or pre-forms
Abstract
The invention discloses a process method for preparing a large-size carbon/carbon heating element, which comprises the following steps: 1) mounting the corundum structural member and the large-size prefabricated body into a resistance type deposition furnace, 2) closing a furnace door, closing a hydrogen and natural gas inlet valve, starting a vacuum pump to vacuumize, and maintaining pressure; 3) heating under negative pressure, controlling the pressure at 3-10KPa and the heating rate at 150 ℃/h until the temperature is increased to 1000 ℃ and 1200 ℃ in the deposition temperature region, and keeping the temperature for 2-10 h; 4) introducing natural gas and hydrogen gas at the same time, wherein the hydrogen gas enters the disc-shaped space through a pipeline and flows into a deposition area of the deposition furnace from the circular hole in the side wall of the disc; 4) introducing nitrogen, and stopping the furnace for cooling. The invention adopts isothermal and isobaric CVI rapid deposition process to prepare the large-size carbon/carbon heating element, has good controllability, high efficiency and low cost, and can be prepared in batch.
Description
Technical Field
The invention relates to a process method for preparing a large-size carbon/carbon heating element.
Background
With the strong demand of the market for new materials such as carbon/carbon composite materials, realizing low-cost and fast-response system supply becomes an urgent necessity to be considered by production suppliers. An effective solution is to increase the charging amount of the medium frequency induction furnace, which means that the sizes of the furnace body and the graphite heating element need to be further increased, but the large-size (diameter larger than 2 m) graphite heating element faces higher processing difficulty and lower yield, which is a pain point in the graphite industry all the time, and in addition, the supply and cost of the large-size graphite raw material are also a factor which cannot be ignored. And the advent of large-sized carbon/carbon heaters became one of the alternatives for equipment suppliers.
And the large-size graphite heating element has poor mechanical property, low strength and poor thermal shock resistance and is easy to break under the action of external force. Because of the limited size of the graphite heating element, the capacity of the medium-frequency induction furnace is always limited, and the charging amount of the medium-frequency induction furnace can be greatly increased by replacing the graphite heating element with the carbon/carbon composite material heating element. The carbon/carbon composite material heating element has the characteristics of high strength, excellent mechanical property, remarkable thermal shock resistance and the like.
The patent "U-shaped carbon/carbon heating element gas phase rapid preparation method" (CN 104710184A), provides a method for preparing carbon/carbon composite material U-shaped heating element, the basic steps are as follows: (1) preparing a graphite core mold; (2) weaving a carbon fiber preform on the basis of the core mold; (3) the method comprises the steps of (1) putting a prefabricated part and a graphite core module assembly into a deposition chamber and connecting the prefabricated part and the graphite core module assembly with an electrode, (4) electrifying the electrode to realize heating, (5) inserting a thermocouple into the prefabricated part, and moving the thermocouple from inside to outside at a specific speed when the temperature of a measured temperature area reaches the deposition temperature; (6) and introducing reaction gas at a certain flow rate after the preset deposition temperature is reached. Processing and forming after gas-phase densification treatment. The patent adopts a thermal gradient CVI process to prepare the carbon/carbon composite material, the preparation of the carbon/carbon composite material depends on a graphite core mold seriously, and the preparation of a large-size carbon/carbon heating body is extremely difficult because the large-size graphite core mold is determined by the characteristics of the graphite core mold tightly attached to a preform, and has the defects of poor mechanical property, low strength, poor density uniformity, uneven current distribution under the condition of electrification, great difference of different deposition parts of the preform and poor controllability.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a process method for preparing a large-size carbon/carbon heating element, which adopts an isothermal and isobaric CVI rapid deposition process to prepare the large-size carbon/carbon heating element, has good controllability, high efficiency and low cost, and can be prepared in batches.
The invention can be solved by the following technical scheme:
a process method for preparing a large-size carbon/carbon heating element comprises the following steps:
1) the method comprises the following steps of installing a corundum structural member and a large-size prefabricated body into a resistance type deposition furnace, wherein the deposition furnace comprises a furnace body, a furnace door, a furnace lining and a heating body, the bottom of the furnace body is provided with two inlets, the horizontal direction is a natural gas inlet, the vertical direction is a hydrogen or nitrogen inlet, and the top of the furnace body is provided with a tail gas outlet; the corundum structural member is divided into an upper part, a middle part and a lower part, wherein the upper part and the lower part are respectively composed of two pieces of corundum, an arc surface-shaped space is formed between the two pieces of corundum, the middle part is two pieces of separated corundum, a disc-shaped space is arranged between the two pieces of corundum, the disc-shaped space is composed of an upper disc and a lower disc, and the side wall of the disc is provided with a round hole;
2) closing the furnace door, closing the hydrogen and natural gas inlet valves, starting a vacuum pump to vacuumize, and maintaining pressure;
3) heating under negative pressure, controlling the pressure at 3-10KPa and the heating rate at 150 ℃/h until the temperature is increased to 1000 ℃ and 1200 ℃ in the deposition temperature region, and keeping the temperature for 2-10 h;
4) introducing natural gas and hydrogen gas at the same time, wherein the hydrogen gas enters the disc-shaped space through a pipeline and flows into a deposition area from the side wall of the disc with the circular hole;
5) introducing nitrogen, and stopping the furnace for cooling.
Wherein the distance formed between the corundum structural member and the large-size prefabricated body is 2-40 mm;
wherein, the upper disc and the lower disc are connected in a matching way through a concave-convex groove.
Wherein the disc-shaped space is arranged at 1/3-1/2 from top to bottom on the total height of the large-size prefabricated body.
Wherein, the upper disc and the lower disc are connected in a matching way through a concave-convex groove.
And 2) when the pressure is pumped to be less than 100Pa in the step 2), the pressure is not changed greatly in 30 minutes, the pressure is maintained for 30-40min, if the pressure rise rate is lower than 20-50Pa/h, the sealing property of the vacuum system meets the requirement, and if the pressure rise rate is larger than the range, the system needs to be checked for leakage.
Wherein the natural gas flow in the step 4) is controlled to be 3-25m3The hydrogen flow rate is preferably controlled to be 0.2 to 1.5m3H is used as the reference value. Wherein, the pressure in the furnace is controlled at 5-25KPa in the step 4), and the deposition time is 150-250 h.
Advantageous effects
The invention can realize the rapid preparation of the carbon/carbon heating element with uniform density by combining the isothermal and isobaric CVI process with the tool, and the carbon/carbon heating element prepared by the method has short process time and uniform deposition density.
Drawings
FIG. 1 is a diagram of a large-sized preform deposition tooling of the present invention;
FIG. 2 is a corundum structural member of the present invention;
FIG. 3 is a disc space of the present invention;
fig. 4 shows the lower half of the disc space of the present invention.
In the drawings
1-furnace body; 2-furnace door; 3-furnace lining; 4-large size preform; 5-corundum structural members; 6-hydrogen inlet; 7-natural gas inlet; 8-a tail gas outlet; 9-heating element.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification.
Example one
A process method for preparing a large-size carbon/carbon heating element comprises the following steps:
1) according to the assembly forming shown in figure 1, the deposition furnace comprises a furnace body 1, a furnace door 2, a furnace lining 3 and a heating element 9, wherein the heating element 9, a large-size prefabricated body 4 and a corundum structural member 5 are arranged on the furnace lining 3, the corundum structural member 5 is arranged in the middle of the furnace body 1, two inlets 6 and 7 are arranged at the bottom of the furnace body 1, a natural gas inlet 7 is arranged in the horizontal direction, a hydrogen or nitrogen inlet 6 is arranged in the vertical direction, and a tail gas outlet is arranged at the top of the furnace body 1; the corundum structural member 5 (shown in figure 2) is divided into an upper part, a middle part and a lower part, wherein the upper part and the lower part are respectively composed of two corundum, an arc-surface-shaped space is formed between the two corundum, the middle part is divided into two separated corundum, a disc-shaped space is arranged between the two corundum, the disc-shaped space is formed by combining an upper disc and a lower disc (the upper disc and the lower disc are connected by matching concave-convex grooves), the side wall of the disc is provided with a circular hole, the distance formed between the corundum structural member 5 and the prefabricated body 4 is controlled to be 2mm, as the corundum structural member has a heat conduction coefficient which is lower than that of a graphite member, as much heat as possible can be controlled between a heating body and a furnace lining, the whole temperature field is more uniform, the isothermal and isobaric CVI process is easier to realize, a layer of graphite paper can be surrounded on the surface of the corundum structural member, a large amount of carbon can be arranged to penetrate into the corundum member to be crisp, in addition, a carbon felt can be arranged in the corundum member, reducing the heat transmitted through the corundum member;
2) closing the furnace door, closing the hydrogen and natural gas inlet valves, starting a vacuum pump to vacuumize, starting pressure maintaining when the pressure is pumped to 100Pa and the pressure change is not large in 10 minutes, keeping the pressure for 30min, wherein if the pressure rise rate is lower than 20Pa/h, the tightness of the vacuum system meets the requirement, and if the pressure rise rate is larger than the range, the system needs to be checked for leakage;
3) heating under negative pressure, controlling the pressure at 3KPa and the heating rate at 100 ℃/h until the temperature rises to 1000 ℃ in a deposition temperature zone, and keeping the temperature for 2 h;
4) opening the valve 7 to introduce natural gas, controlling the flow rate of the natural gas at 3m3At the same time, the valve 6 is opened to introduce hydrogen, which is introduced into a disk-shaped space through a pipeline (as shown in FIGS. 3 and 4), and the hydrogen flows into the deposition area from the side wall of the disk with the circular holes, and the flow rate is controlled to be 0.2m3The disc space is located at 1/3 of the total height of the preform. The purpose of introducing hydrogen is to inhibit the generation of macromolecular substances, the microstructure of CVI pyrolytic carbon is controlled by adjusting the volume fraction of hydrogen in gas-phase components, and the pressure in the furnace is controlled at 5 KPa. The deposition time is 150 h;
5) introducing nitrogen, and stopping the furnace for cooling.
Example two
A process method for preparing a large-size carbon/carbon heating element comprises the following steps:
1) according to the assembly forming shown in figure 1, the deposition furnace comprises a furnace body 1, a furnace door 2, a furnace lining 3 and a heating element 9, wherein the heating element 9, a large-size prefabricated body 4 and a corundum structural member 5 are arranged on the furnace lining 3, the corundum structural member 5 is arranged in the middle of the furnace body 1, two inlets 6 and 7 are arranged at the bottom of the furnace body 1, a natural gas inlet 7 is arranged in the horizontal direction, a hydrogen or nitrogen inlet 6 is arranged in the vertical direction, and a tail gas outlet is arranged at the top of the furnace body 1; the corundum structural member 5 (shown in figure 2) is divided into an upper part, a middle part and a lower part, wherein the upper part and the lower part are respectively composed of two corundum, an arc-surface-shaped space is formed between the two corundum, the middle part is divided into two separated corundum, a disc-shaped space is arranged between the two corundum, the disc-shaped space is formed by combining an upper disc and a lower disc (the upper disc and the lower disc are connected by matching concave-convex grooves), the side wall of the disc is provided with a circular hole, the distance formed between the corundum structural member 5 and the prefabricated body 4 is controlled to be 40mm, as the corundum structural member has a heat conduction coefficient which is lower than that of a graphite member, as much heat as possible can be controlled between a heating body and a furnace lining, the whole temperature field is more uniform, the isothermal and isobaric CVI process is easier to realize, a layer of graphite paper can be surrounded on the surface of the corundum structural member, a large amount of carbon can be arranged to penetrate into the corundum member to be crisp, in addition, a carbon felt can be arranged in the corundum member, reducing the heat transmitted through the corundum member;
2) closing the furnace door, closing the hydrogen and natural gas inlet valves, starting a vacuum pump to vacuumize, starting pressure maintaining when the pressure is pumped to 80Pa and the pressure change is not large in 10 minutes, keeping the pressure for 40min, wherein if the pressure rise rate is lower than 50Pa/h, the tightness of the vacuum system meets the requirement, and if the pressure rise rate is larger than the range, the system needs to be checked for leakage;
3) heating under negative pressure, controlling the pressure at 10KPa and the heating rate at 150 ℃/h until the temperature rises to 1200 ℃ of a deposition temperature zone, and preserving the heat for 10 h;
4) opening the valve 7 to introduce natural gas, wherein the flow rate of the natural gas is controlled to be 25m3At the same time, the valve 6 is opened to introduce hydrogen, which is introduced into a disk-shaped space through a pipe (as shown in FIGS. 3 and 4), and the hydrogen flows into the deposition region from the side wall of the disk with the circular holes, and the flow rate is preferably controlled to be 1.5m3The disc space is located at 1/2 of the total height of the preform. The purpose of introducing hydrogen is to inhibit the generation of macromolecular substances, the microstructure of CVI pyrolytic carbon is controlled by adjusting the volume fraction of hydrogen in gas-phase components, and the pressure in the furnace is controlled at 25 KPa. The deposition time is 250 h;
5) introducing nitrogen, and stopping the furnace for cooling.
EXAMPLE III
A process method for preparing a large-size carbon/carbon heating element comprises the following steps:
1) according to the assembly forming shown in figure 1, the deposition furnace comprises a furnace body 1, a furnace door 2, a furnace lining 3 and a heating element 9, wherein the heating element 9, a large-size prefabricated body 4 and a corundum structural member 5 are arranged on the furnace lining 3, the corundum structural member 5 is arranged in the middle of the furnace body 1, two inlets 6 and 7 are arranged at the bottom of the furnace body 1, a natural gas inlet 7 is arranged in the horizontal direction, a hydrogen or nitrogen inlet 6 is arranged in the vertical direction, and a tail gas outlet is arranged at the top of the furnace body 1; the corundum structural member 5 (shown in figure 2) is divided into an upper part, a middle part and a lower part, wherein the upper part and the lower part are respectively composed of two corundum, an arc-surface-shaped space is formed between the two corundum, the middle part is two separated corundum, a disc-shaped space is arranged between the two corundum, the disc-shaped space is formed by combining an upper disc and a lower disc (the upper disc and the lower disc are connected by matching concave-convex grooves), the side wall of the disc is provided with a circular hole, the distance formed between the corundum structural member 5 and the prefabricated body 4 is preferably controlled to be 20mm, as the corundum structural member has a heat conduction coefficient which is lower than that of a graphite member, as much heat as possible can be controlled between a heating body and a furnace lining, the whole temperature field is more uniform, the isothermal and isobaric CVI process is easier to realize, a layer of graphite paper can be surrounded on the surface of the corundum structural member, a large amount of carbon can be deeply deposited inside the corundum member to be embrittled, besides, a carbon felt can be placed inside the corundum member, reducing the heat transmitted through the corundum member;
2) closing the furnace door, closing the hydrogen and natural gas inlet valves, starting a vacuum pump to vacuumize, starting pressure maintaining for 35min when the pressure is pumped to 60Pa and the pressure change is not large in 10 minutes, wherein if the pressure rise rate is lower than 25Pa/h, the sealing property of the vacuum system meets the requirement, and if the pressure rise rate is larger than the range, the system needs to be checked for leakage;
3) heating under negative pressure, controlling the pressure at 6KPa and the heating rate at 120 ℃/h until the temperature rises to 1100 ℃ in a deposition temperature zone, and keeping the temperature for 6 h;
4) opening the valve 7 to feed natural gas, wherein the flow rate of the natural gas is controlled to be 12m3At the same time, the valve 6 is opened to introduce hydrogen, which is introduced into a disk-shaped space through a pipeline (as shown in FIGS. 3 and 4), and the hydrogen flows into the deposition area from the side wall of the disk with the circular holes, and the flow rate is controlled to be 1.2m3The disc space is located at 5/12 of the total height of the preform. The purpose of introducing hydrogen is to inhibit the generation of macromolecular substances, the microstructure of CVI pyrolytic carbon is controlled by adjusting the volume fraction of hydrogen in gas-phase components, and the pressure in the furnace is preferably controlled at 15 KPa. The deposition time is 180 h;
5) introducing nitrogen, and stopping the furnace for cooling.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (7)
1. A process method for preparing a large-size carbon/carbon heating element is characterized by comprising the following steps:
1) the method comprises the following steps of installing a corundum structural member and a large-size prefabricated body into a resistance type deposition furnace, wherein the deposition furnace comprises a furnace body, a furnace door, a furnace lining and a heating body, the bottom of the furnace body is provided with two inlets, the horizontal direction is a natural gas inlet, the vertical direction is a hydrogen or nitrogen inlet, and the top of the furnace body is provided with a tail gas outlet; the corundum structural member is divided into an upper part, a middle part and a lower part, wherein the upper part and the lower part are respectively composed of two pieces of corundum, an arc surface-shaped space is formed between the two pieces of corundum, the middle part is two pieces of separated corundum, a disc-shaped space is arranged between the two pieces of corundum, the disc-shaped space is composed of an upper disc and a lower disc, and the side wall of the disc is provided with a round hole;
2) closing the furnace door, closing the hydrogen and natural gas inlet valves, starting a vacuum pump to vacuumize, and maintaining pressure;
3) heating under negative pressure, controlling the pressure at 3-10KPa and the heating rate at 150 ℃/h until the temperature is increased to 1000 ℃ and 1200 ℃ in the deposition temperature region, and keeping the temperature for 2-10 h;
4) introducing natural gas and hydrogen gas at the same time, wherein the hydrogen gas enters the disc-shaped space through a pipeline and flows into a deposition area of the deposition furnace from the circular hole in the side wall of the disc;
5) introducing nitrogen, and stopping the furnace for cooling.
2. A process according to claim 1, wherein the corundum structure is at a distance of 2-40mm from the large-size preform.
3. The process of claim 1 wherein said upper and lower disks are joined by a tongue and groove fit.
4. The process of claim 1, wherein the disc-shaped space is provided at 1/3-1/2 from top to bottom of the total height of the large-size preform.
5. The process of claim 1, wherein in step 2), when the pressure is reduced to below 100Pa and the pressure does not change greatly in 30 minutes, the pressure is maintained for 30-40 min.
6. The process of claim 1, wherein the natural gas flow rate in step 4) is controlled to be 3-25m3The hydrogen flow is controlled between 0.2 and 1.5m3/h。
7. The process as claimed in claim 1, wherein the pressure in the furnace in step 4) is controlled at 5-25KPa, and the deposition time is 150-250 h.
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