CN115872766A - Preparation method of carbon-carbon material heat preservation device and heat preservation device - Google Patents
Preparation method of carbon-carbon material heat preservation device and heat preservation device Download PDFInfo
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Abstract
The application discloses this application belongs to heat preservation device and makes technical field, especially relates to a preparation method and heat preservation device of carbon-carbon material heat preservation device. The preparation method comprises the following steps: providing an end blank; providing a middle blank body, wherein the middle blank body is formed by dipping a prefabricated blank body by a curing impregnant, and then sequentially carrying out hot-press forming, carbonization, first chemical vapor deposition, heat treatment, processing and shaping and second chemical vapor deposition, the hot-press forming is carried out in a closed environment, the temperature is raised to 150-300 ℃, and the heat is preserved for 2-5 hours; and bonding the end part blank body and the middle part blank body to obtain the heat preservation device. The hot-air pressing molding is performed before carbonization and chemical vapor deposition, so that the strength uniformity and the thickness uniformity of the material are fully improved, and the manufactured heat preservation device has high and uniform strength and is not easy to damage; the prefabricated blank can be added with a fiber reinforcement, so that the thermal shock resistance is improved, and the heat-resisting and heat-insulating properties are improved.
Description
Technical Field
The application belongs to the technical field of heat preservation device manufacturing, and particularly relates to a preparation method of a carbon-carbon material heat preservation device and the heat preservation device.
Background
In the prior art, a thermal field assembly is required in the crystal growth process, and the performance of the thermal field assembly directly influences the crystal growth. For example, the thermal insulating barrel is an important thermal field component for melting raw materials in the crystal growth process.
The size of the furnace body of the existing single crystal furnace is larger, the size of the heat-insulating cylinder is increased along with the size of the heat-insulating cylinder, the size of equipment for producing the heat-insulating cylinder is increased, the cost and the requirement of the existing equipment for producing the heat-insulating cylinder are increased gradually, the utilization rate of the furnace body is low, and the production cost is high.
On the other hand, the size of the traditional heat-insulating cylinder is difficult to control in the weaving process, so that a large amount of processing allowance is required to be reserved, and the actual utilization rate of the woven body and the heat-insulating cylinder is only 50-70%.
Disclosure of Invention
The embodiment of the application provides a preparation method of a carbon-carbon material heat preservation device and the heat preservation device, and aims to provide a preparation method of the heat preservation device which is excellent in performance and low in cost.
In one aspect, the application provides a method for preparing a carbon-carbon material heat preservation device, comprising the following steps:
providing an end blank;
providing a middle blank body, wherein the middle blank body is formed by dipping a prefabricated blank body by a curing impregnant, and then sequentially carrying out hot-press forming, carbonization, first chemical vapor deposition, heat treatment, processing and shaping and second chemical vapor deposition, the hot-press forming is carried out in a closed environment, the temperature is raised to 150-300 ℃, and the heat is preserved for 2-5 hours;
and bonding the end part blank body and the middle part blank body to obtain the heat preservation device.
Optionally, the components of the curing impregnant include a phenolic resin, a furfural resin, or a combination thereof;
the curing impregnant also comprises graphite powder and alcohol.
Optionally, the initial pressure of the hot-air pressing is 0.5MPA-9MPA; and/or the presence of a gas in the gas,
the heating rate of the hot-air pressing molding is 10-20 ℃/min.
Optionally, the carbonization temperature is 900-1200 ℃, and the time is 2-10h.
Optionally, the carbonized density is 0.8-1.2g/cm dry harvested.
Optionally, the temperature of the first chemical vapor deposition is 1000 ℃ to 1200 ℃, and the furnace pressure of the first chemical vapor deposition is 3000pa to 5000pa.
Optionally, the density after the first chemical vapor deposition is between 1.3 and 1.5 g/cm.
Optionally, the temperature of the heat treatment is 1500-2000 ℃, and the time of the heat treatment is 5-10 h.
Optionally, the temperature of the second chemical vapor deposition is 1100 ℃ to 1200 ℃, and the furnace pressure of the second chemical vapor deposition is 500pa to 1000pa.
In a second aspect, the present application provides a spliced insulation device obtained by the method of the first aspect.
According to the preparation method of the carbon-carbon material heat preservation device, the end part blank body and the middle part blank body are bonded, waste of traditional materials is avoided, the utilization rate is only 50-70%, and the material utilization rate of the heat preservation device prepared by the method reaches more than 85%. Providing a middle blank body, wherein the middle blank body is formed by dipping a prefabricated blank body by a curing impregnant, and then sequentially carrying out hot-press forming, carbonization, first chemical vapor deposition, heat treatment, processing and shaping and second chemical vapor deposition, the hot-press forming is carried out in a closed environment, the temperature is raised to 150-300 ℃, and the heat is preserved for 2-5 hours; the hot-air pressing molding is performed before carbonization and chemical vapor deposition, so that the strength uniformity and the thickness uniformity of the material are fully improved, and the manufactured heat preservation device has high and uniform strength and is difficult to damage, and is about 10 times of graphite; the prefabricated blank can be added with a fiber reinforcement, so that the thermal shock resistance is improved, and the heat resistance and heat preservation performance are improved; because form through segmentation processing and concatenation, the structure is special, difficult deformation: absorbing thermal stress and reducing thermal deformation, thereby improving the hot creep resistance.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of a carbon-carbon material heat preservation device provided in an embodiment of the present application.
Detailed Description
Features and exemplary embodiments of various aspects of the present application will be described in detail below, and in order to make the objects, technical solutions and advantages of the present application more apparent, the present application will be further described in detail below with reference to specific embodiments. It should be understood that the specific embodiments described herein are intended to be illustrative only and are not intended to be limiting. It will be apparent to one skilled in the art that the present application may be practiced without some of these specific details. The following description of the embodiments is merely intended to provide a better understanding of the present application by illustrating examples thereof.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrases "comprising 8230; \8230;" 8230; "does not exclude the presence of additional like elements in a process, method, article, or apparatus that comprises the element.
Preparation method of carbon-carbon material heat preservation device
In a first aspect, the present application provides a method for preparing a carbon-carbon material heat preservation device, as shown in fig. 1, including:
s1, providing an end part blank;
in this embodiment, the end blank may be formed from the end preform by vapor deposition, carbonization, elevated temperature, work setting, and vapor deposition.
S2, providing a middle blank body, wherein the middle blank body is formed by sequentially carrying out hot-air forming, carbonization, first chemical vapor deposition, heat treatment, processing and shaping and second chemical vapor deposition after a prefabricated blank body is impregnated by a curing impregnant, and the hot-air forming is carried out in a closed environment, the temperature is raised to 150-300 ℃, and the heat is preserved for 2-5 hours;
in this embodiment, the preform may be formed by alternately laminating and needling a carbon fiber mesh, a carbon cloth, and carbon fiber filaments into a desired size, or may be formed by mechanically pressing a straight plate into an arc shape. The shape of the prefabricated blank is not limited, and the prefabricated blank can be in a straight plate shape, an arc shape and the like, is determined according to the target shape of the heat preservation device, and can also be adjusted for simple and convenient subsequent processing procedures.
And S3, bonding the end part blank body and the middle part blank body to obtain the heat preservation device.
In this embodiment, the entire heat-retaining device can be obtained by performing bonding by sewing or the like, and impregnating, vapor-depositing, and carbonizing the bonded portion. The end part blank body and the middle part blank body can be sewed to the inner layer of the needled felt through quartz fiber threads; and then, using impregnation liquid to perform semi-curing impregnation, and finally matching with other processes to perform co-curing compounding.
According to the embodiment of the application, the middle blank of the end blank is formed by bonding, the waste of traditional materials is avoided, the utilization rate is only 50-70%, and the utilization rate of the material of the heat preservation device manufactured by the method reaches more than 85%. Providing a middle blank body, wherein the middle blank body is formed by dipping a prefabricated blank body by a curing impregnant, and then sequentially carrying out hot-press forming, carbonization, first chemical vapor deposition, heat treatment, processing and shaping and second chemical vapor deposition, the hot-press forming is carried out in a closed environment, the temperature is raised to 150-300 ℃, and the heat is preserved for 2-5 hours; the hot-air pressing molding is performed before carbonization and chemical vapor deposition, so that the strength uniformity and the thickness uniformity of the material are fully improved, and the manufactured heat preservation device has high and uniform strength and is difficult to damage, and is about 10 times of graphite; because form through segmentation processing and concatenation, the structure is special, difficult deformation: absorbing thermal stress and reducing thermal deformation, thereby improving the hot creep resistance.
In some embodiments, fiber reinforcement may also be added to the pre-formed embryo body. Has the functions of improving the thermal shock resistance and the heat-resisting and heat-preserving performance.
In some embodiments, the component of the curing impregnant includes a phenolic resin, a furfural resin, or a combination thereof. The phenolic resin and the furfural resin can be filled in the gaps of the prefabricated blanks, the density and the carbon content between the heat preservation devices are improved, the crosslinking performance is improved, the heat preservation and the high temperature resistance are improved,
in some embodiments, the curing impregnant further includes graphite powder and alcohol. The graphite powder in the curing impregnant can be added and filled in the gaps of the prefabricated blank body, and the alcohol can dissolve phenolic resin and furfural resin, so that the cross-linking property and the nucleation property of the graphite powder and the prefabricated blank body at high temperature are improved.
In some embodiments, the initial pressure of the hot air press molding is 0.5MPA to 9MPA. The initial pressure is controlled in a lower range, so that oxygen in hot-air pressure forming can be discharged, and the interference of reaction gas such as oxygen can be avoided. Meanwhile, the effect of air pressure forming is improved, and the uniformity of the blank body after air pressure forming is improved.
It should be noted that, after the prefabricated blank coated with the curing impregnant is placed into the hot-press forming mold and before the prefabricated blank is placed into the hot-press furnace, the hot-press forming mold needs to be vacuumized, so that the interference of oxygen and the like which can generate reaction gas is avoided.
In some embodiments, the heating rate of the hot-air pressing is 10-20 ℃/min. The heating speed of the air pressure forming is controlled, so that the heating uniformity is kept, the temperature uniformity of the whole blank is controlled, the uniformity of the structure of the heat preservation device in the thickness direction is promoted, and the uniform heat preservation performance and the uniform strength of the heat preservation device are improved. The uniformity of strength can be further improved, and the airtightness is stable.
In some embodiments, the carbonization is performed at a temperature of 900 ℃ to 1200 ℃ for 2 to 10 hours. The carbonization temperature is controlled, the densification speed and the pyrolytic carbon structure can be adjusted, and the preset carbonization effect is achieved.
In some embodiments, the post-carbonization density is 0.8-1.2g/cm ethanol.
In some embodiments, the temperature of the first chemical vapor deposition is 1000 ℃ to 1200 ℃, and the furnace pressure of the first chemical vapor deposition is 3000pa to 5000pa. The densification speed and the pyrolytic carbon structure can be adjusted by controlling the temperature and the furnace pressure of vapor deposition.
In some embodiments, the density is between 1.3 and 1.5g/cm following the first chemical vapor deposition.
In some embodiments, the temperature of the heat treatment is 1500 ℃ to 2000 ℃ and the time of the heat treatment is 5h to 10h. The density can be improved by controlling the temperature and time of the heat treatment, so that the alloy has high strength and good air tightness.
In some embodiments, the temperature of the second chemical vapor deposition is 1100 ℃ to 1200 ℃, and the furnace pressure of the second chemical vapor deposition is 500pa to 1000pa. The densification speed and the pyrolytic carbon structure can be adjusted by controlling the temperature and the furnace pressure of vapor deposition, the density can be improved, and the high-strength high-tightness high-density thermal decomposition furnace has high strength and good air tightness.
Heat preservation device
In a second aspect, the present application provides a spliced insulation device obtained by the method of the first aspect. The heat preservation device of this application can be for the heat-preserving container of cylinder, rectangular bodily form's insulation can etc. can design according to the demand.
The heat preservation device prepared by the method is applied to a high-temperature furnace thermal field and has the characteristics of high strength, long service life, environmental protection, energy conservation and the like. The thermal field does not need to be modified, and the adaptability is high; the thermal conductivity is about 1/2 to 1/5 of that of graphite. The bending strength is more than 130 MPa, and the thermal conductivity is 4 to 10W/(m.k). In some embodiments, the density of the holding device is between 1.29 and 1.35 g/cm.
Examples
The present disclosure is more particularly described in the following examples that are intended as illustrative only, since various modifications and changes within the scope of the present disclosure will be apparent to those skilled in the art. All parts, percentages, and ratios reported in the following examples are on a weight basis, all reagents used in the examples are commercially available or synthesized according to conventional methods and can be used directly without further treatment, and the equipment used in the examples is commercially available, unless otherwise specified.
The phenolic resin was obtained from model ZL3000 from Sienna Yue Biotechnology, inc.
Example 1
The embodiment provides a preparation method of a carbon-carbon material heat preservation device, which comprises the following steps:
providing a middle blank body, wherein the middle blank body is formed by dipping a prefabricated blank body by a curing impregnant, and then sequentially carrying out hot-press forming, carbonization, first chemical vapor deposition, heat treatment, processing and shaping and second chemical vapor deposition, the hot-press forming is carried out in a closed environment, the temperature is raised to 200 ℃, and the heat is preserved for 3 hours;
the middle blank body is arc-shaped, and the process comprises the following steps:
1) Preparing a curing impregnant: the phenolic resin, graphite powder and alcohol are mixed and stirred according to a proportion, the stirring process comprises the steps of firstly mixing and stirring the resin and the alcohol uniformly according to a proportion of 8. The stirring speed is 1-5 r/s, and the stirring time is 12-24h.
2) Preparing a prefabricated blank body: the straight plate (not cured) is pressed into an arc shape at normal temperature by a mechanical press. The process uses a small pressure, but presses the straight plates into roughly similar shapes, without producing a compressive load.
3) And uniformly coating the surface of the prefabricated blank after cold pressing with the prepared curing impregnant for coating by 3mm.
4) After the coating is finished, the arc-shaped plate is placed into a polyether ketone plastic bag, and the polyether ketone plastic bag is vacuumized and then placed into an air pressure mold.
5) And (3) loading a mold, putting the mold into a hot pressing furnace, slowly increasing the pressure to 6MPA, slowly increasing the temperature to 200 ℃ after the pressure reaches specified parameters, and preserving the temperature for 3.5 hours.
6) Slowly cooling, discharging and locking the die.
7) And putting the pressed die and the product into a carbonization furnace together, slowly heating to 1000 ℃, and carrying out carbonization for 8 hours until the density reaches between 1.0g/cm for carbonization after the carbonization is discharged from the furnace.
8) And (3) carrying out chemical vapor deposition (CVI) on the carbonized product at the temperature of 1100 ℃, under the furnace pressure of 4000pa, and enabling the density of the discharged product to reach 1.4.
9) High-temperature treatment: the temperature is 1800 ℃ and the time is 7h.
10 Processing and shaping: machining to a specified shape.
11 CVI) at 1150 c, furnace pressure 800pa.
Providing an end blank; wherein, the end part blank is a circular arc section blank, and the process is as follows:
1) And carrying out chemical vapor deposition on the prefabricated blank of the arc section at the temperature of 1100 ℃, under the furnace pressure of 4000pa, and enabling the density to reach 0.85 after discharging.
2) Post-impregnation: asphalt is used for impregnation. And previous product type
3) Carrying out carbon: slowly heating to 1100 ℃, keeping the time for 8 hours, carbonizing, and taking the carbonized product out of the furnace until the density reaches 1.4g/cm during the year of double cropping.
4) High-temperature treatment: the temperature is 1800 ℃ and the time is 7h.
5) And (5) processing and shaping, namely, machining to a specified shape.
6) Carrying out chemical vapor deposition at 1150 ℃, furnace pressure of 700pa and density of 1.30g/cm for carrying out the high-speed thin film transistor liquid crystal growing. And bonding the end part blank body and the middle part blank body to obtain the heat-insulating barrel.
Example 2
The embodiment provides a preparation method of a carbon-carbon material heat preservation device, which comprises the following steps:
providing a middle blank body, wherein the middle blank body is formed by dipping a prefabricated blank body by a curing impregnant, and then sequentially carrying out hot-press forming, carbonization, first chemical vapor deposition, heat treatment, processing and shaping and second chemical vapor deposition, the hot-press forming is carried out in a closed environment, the temperature is raised to 150 ℃, and the heat is preserved for 2 hours;
the middle blank body is arc-shaped, and the process comprises the following steps:
1) Preparing a curing impregnant: the phenolic resin, graphite powder and alcohol are mixed and stirred according to a ratio, the stirring process comprises the steps of mixing and stirring the resin and the alcohol uniformly according to a ratio of 8. The stirring speed is 1-5 r/s, and the stirring is carried out for 12-24h.
2) Preparing a prefabricated blank body: the straight plate (not cured) is pressed into an arc shape at normal temperature by a mechanical press. The process uses a small pressure, but presses the straight plates into roughly similar shapes, without producing a compressive load.
3) Uniformly coating the surface of the prefabricated blank after cold pressing with the prepared curing impregnant, wherein the coating is 1-5mm.
4) After the coating is finished, the arc-shaped plate is placed into a polyether ketone plastic bag, and the polyether ketone plastic bag is vacuumized and placed into an air pressure mold.
5) And (3) loading a mold, putting the mold into a hot pressing furnace, slowly increasing the pressure to 0.5MPA, slowly increasing the temperature to 150 ℃ after the pressure reaches specified parameters, and preserving the heat for 2 hours.
6) Slowly cooling, discharging and locking the die.
7) And putting the pressed die and the product into a carbonization furnace together, slowly heating to 900 ℃, and carrying out carbonization for 4 hours until the density reaches between 0.8g/cm for carbonization after discharge.
8) After carbonization, the product is subjected to chemical vapor deposition (CVI) at a temperature of 1000 ℃, and performing furnace pressure of 3000pa, and performing high-density cultivation after discharging until the density reaches 1.3 g/cm.
9) High-temperature treatment: the temperature is 1500 ℃, and the time is 5h.
10 Processing and shaping: machining to a specified shape.
11 CVI, temperature 1100 ℃ oven pressure 500pa.
Providing an end blank; wherein, the end part blank is a circular arc section blank, and the process is as follows:
1) Carrying out chemical vapor deposition on the prefabricated blank of the arc section at the temperature of 1000 ℃, and performing furnace pressure of 3000pa, and performing high-density cultivation after discharging until the density reaches 0.7 g/cm.
2) Post-impregnation: asphalt is used for impregnation. And previous product type
3) Carrying out carbon: slowly heating to 900 ℃, carrying out carbonization for 2 hours, and carrying out carbonization and discharging until the density reaches 1.3g/cm for carrying out thin film crop.
4) High-temperature treatment: the temperature is 1500 ℃, and the time is 5h.
5) And (5) processing and shaping, namely, machining to a specified shape.
6) Performing chemical vapor deposition at 1100 deg.C under 500pa with density of 1.295 g/cm.
And bonding the end part blank body and the middle part blank body to obtain the heat-insulating barrel.
The rest is the same as example 1.
Example 3
The embodiment provides a preparation method of a carbon-carbon material heat preservation device, which comprises the following steps:
providing a middle blank body, wherein the middle blank body is formed by dipping a prefabricated blank body by a curing impregnant, and then sequentially carrying out hot-press forming, carbonization, first chemical vapor deposition, heat treatment, processing and shaping and second chemical vapor deposition, the hot-press forming is carried out in a closed environment, the temperature is raised to 300 ℃, and the heat is preserved for 5 hours;
the middle blank body is arc-shaped, and the process comprises the following steps:
1) Preparing a curing impregnant: the phenolic resin, graphite powder and alcohol are mixed and stirred according to a proportion, the stirring process comprises the steps of firstly mixing and stirring the resin and the alcohol uniformly according to a proportion of 8. The stirring speed is 1-5 r/s, and the stirring is carried out for 12-24h.
2) Preparing a prefabricated blank body: the straight plate (not cured) is pressed into an arc shape at normal temperature by a mechanical press. The process uses a small pressure, but presses the straight plates into roughly similar shapes, without producing a compressive load.
3) Uniformly coating the surface of the prefabricated blank after cold pressing with the prepared curing impregnant, wherein the coating is 1-5mm.
4) After the coating is finished, the arc-shaped plate is placed into a polyether ketone plastic bag, and the polyether ketone plastic bag is vacuumized and then placed into an air pressure mold.
5) And (3) loading a mold, putting the mold into a hot pressing furnace, slowly increasing the pressure to 9MPA, slowly increasing the temperature to 300 ℃ after the pressure reaches specified parameters, and preserving the temperature for 5 hours.
6) Slowly cooling, discharging and locking the die.
7) And putting the pressed die and the product into a carbonization furnace, slowly heating to 1200 ℃, and carrying out carbonization for 2-10 hours until the density reaches between 1.2g/cm for carbonization after discharge.
8) After carbonization, the product is subjected to chemical vapor deposition (CVI) at the temperature of 1200 ℃, and (5) performing furnace pressure of 5000pa, and performing high-density cultivation after discharging until the density reaches 1.5 g/cm.
9) High-temperature treatment: the temperature is 2000 ℃, and the time is 10h.
10 Processing and shaping: machining to a specified shape.
11 CVI, temperature 1200 ℃ and furnace pressure 1000pa.
Providing an end blank; wherein, the end part blank is a circular arc section blank, and the process is as follows:
1) Carrying out chemical vapor deposition on the prefabricated blank of the arc section at the temperature of 1200 ℃, and (5) performing furnace pressure of 5000pa, and performing high-density cultivation after discharging until the density reaches 1.0 g/cm.
2) Post-impregnation: asphalt is used for impregnation. And previous product type
3) Carrying out carbon: slowly heating to 900-1200 ℃, carrying out carbonization for 2-10h, and carrying out thin film tube rolling on the obtained product, wherein the carbonization density reaches 1.5g/cm after the carbonization is discharged from the furnace.
4) High-temperature treatment: the temperature is 2000 ℃, and the time is 10h.
5) And (5) processing and shaping, namely, machining to a specified shape.
6) Performing chemical vapor deposition at 1200 deg.C under 1000pa, and harvesting at density of 1.31 g/cm.
And bonding the end part blank body and the middle part blank body to obtain the heat-insulating barrel.
The rest is the same as example 1.
Comparative example 1
The preform was directly formed into a predetermined shape of a heat-insulating barrel, and subjected to conventional vapor deposition and carbonization, otherwise the same as in example 1.
Performance testing
Density detection is carried out on 5 parts at the middle end of the heat-preserving barrel by using a method of density and concentration measurement Lixing, and the mean value is taken;
using a GB/T34559-2017 carbon/carbon composite material compression performance test method to detect the bending strength of 5 parts at the middle end of the heat-insulating barrel, and taking an average value;
and (3) detecting the uniformity of the strength by using a GB/T34559-2017 carbon/carbon composite material compression performance test method, and judging that the composite material is not uniform when the strength difference is greater than 8 Mpa.
And (3) detecting the heat conductivity coefficients of 5 parts at the middle end of the heat-insulating barrel by using a GB/T8722-2019 method, and taking an average value.
The binders of examples 1 to 3 and comparative examples 1 to 2 were tested, and the tested structures are shown in table 3.
| Item | Example 1 | Example 2 | Example 3 | Comparative example 1 |
| High density g/cm | 1.68 | 1.70 | 1.69 | 1.61 |
| Bending strengthMPa | 1452 | 1451 | 1456 | 1328 |
| Uniformity of bending strength | Uniformity | Uniformity | Uniformity | Unevenness of |
| Thermal conductivity W/(m.k) | 5 | 6 | 5.8 | 23 |
The heat preservation device has the density of more than 1.65g/cm, the bending strength of more than 1450MPa, the heat conductivity of 4 to 10W/(m.k), the strength is more uniform, and the heat preservation performance is better.
It should also be noted that the exemplary embodiments mentioned in this application describe some methods or systems based on a series of steps or devices. However, the present application is not limited to the order of the above steps, that is, the steps may be performed in the order mentioned in the embodiments, may be performed in an order different from the order in the embodiments, or may be performed at the same time.
As described above, only the specific embodiments of the present application are provided, and it can be clearly understood by those skilled in the art that, for convenience and brevity of description, the specific working processes of the system, the module and the unit described above may refer to the corresponding processes in the foregoing method embodiments, and are not described herein again. It should be understood that the scope of the present application is not limited thereto, and any person skilled in the art can easily conceive various equivalent modifications or substitutions within the technical scope of the present application, and these modifications or substitutions should be covered within the scope of the present application.
Claims (10)
1. A preparation method of a carbon-carbon material heat preservation device comprises the following steps:
providing an end blank;
providing a middle blank body, wherein the middle blank body is formed by dipping a prefabricated blank body by a curing impregnant, and then sequentially carrying out hot-press forming, carbonization, first chemical vapor deposition, heat treatment, processing and shaping and second chemical vapor deposition, the hot-press forming is carried out in a closed environment, the temperature is raised to 150-300 ℃, and the heat is preserved for 2-5 hours;
and bonding the end part blank body and the middle part blank body to obtain the heat preservation device.
2. The method of claim 1, wherein the components of the curing impregnant include phenolic resins, furfural resins, or combinations thereof;
the curing impregnant also comprises graphite powder and alcohol.
3. The method as claimed in claim 1, wherein the hot press molding is performed at an initial pressure of 0.5MPA to 9MPA; and/or the presence of a gas in the gas,
the heating rate of the hot-air pressing molding is 10-20 ℃/min.
4. The method according to claim 1, wherein the carbonization is carried out at 900-1200 ℃ for 2-10h.
5. Preparation method according to claim 1, wherein the density after carbonization is between 0.8 and 1.2 g/cm.
6. The method according to claim 1, wherein the temperature of the first chemical vapor deposition is 1000 ℃ to 1200 ℃, and the furnace pressure of the first chemical vapor deposition is 3000pa to 5000pa.
7. The method of claim 1, wherein the first cvd is followed by a density of 1.3-1.5 g/cm.
8. The method for preparing the alloy material according to claim 1, wherein the temperature of the heat treatment is 1500 ℃ to 2000 ℃ and the time of the heat treatment is 5h to 10h.
9. The method according to any one of claims 1 to 8, wherein the temperature of the second chemical vapor deposition is 1100 ℃ to 1200 ℃, and the furnace pressure of the second chemical vapor deposition is 500pa to 1000pa.
10. A spliced thermal insulation device obtained by the production method according to any one of claims 1 to 9.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11255587A (en) * | 1998-03-12 | 1999-09-21 | Sumitomo Metal Ind Ltd | Carbon-fiber reinforced carbonaceous material crucible for pulling single crystal and its production |
| CN103342572A (en) * | 2012-08-15 | 2013-10-09 | 山东伟基炭科技有限公司 | Method of preparing C/C composite material |
| CN112047749A (en) * | 2020-07-29 | 2020-12-08 | 株洲红亚电热设备有限公司 | Carbon-carbon crucible, manufacturing method and induction heating furnace |
| CN112341232A (en) * | 2020-10-28 | 2021-02-09 | 西安超码科技有限公司 | Carbon/carbon crucible and manufacturing method thereof |
| CN113024269A (en) * | 2021-03-19 | 2021-06-25 | 中南大学 | Preparation method of high-performance super-large and super-thick carbon/carbon composite material |
| CN113151893A (en) * | 2021-04-29 | 2021-07-23 | 上海骐杰碳素材料有限公司 | Fiber bowl-shaped preform, carbon-carbon bowl body and crucible comprising same |
| CN113845369A (en) * | 2021-10-29 | 2021-12-28 | 西安美兰德新材料有限责任公司 | Production process of plate for carbon spliced heat-insulation cylinder |
| CN113860900A (en) * | 2021-10-29 | 2021-12-31 | 西安美兰德新材料有限责任公司 | Rapid preparation method of high-performance carbon fiber composite material plate |
-
2022
- 2022-11-14 CN CN202211419482.5A patent/CN115872766B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11255587A (en) * | 1998-03-12 | 1999-09-21 | Sumitomo Metal Ind Ltd | Carbon-fiber reinforced carbonaceous material crucible for pulling single crystal and its production |
| CN103342572A (en) * | 2012-08-15 | 2013-10-09 | 山东伟基炭科技有限公司 | Method of preparing C/C composite material |
| CN112047749A (en) * | 2020-07-29 | 2020-12-08 | 株洲红亚电热设备有限公司 | Carbon-carbon crucible, manufacturing method and induction heating furnace |
| CN112341232A (en) * | 2020-10-28 | 2021-02-09 | 西安超码科技有限公司 | Carbon/carbon crucible and manufacturing method thereof |
| CN113024269A (en) * | 2021-03-19 | 2021-06-25 | 中南大学 | Preparation method of high-performance super-large and super-thick carbon/carbon composite material |
| CN113151893A (en) * | 2021-04-29 | 2021-07-23 | 上海骐杰碳素材料有限公司 | Fiber bowl-shaped preform, carbon-carbon bowl body and crucible comprising same |
| CN113845369A (en) * | 2021-10-29 | 2021-12-28 | 西安美兰德新材料有限责任公司 | Production process of plate for carbon spliced heat-insulation cylinder |
| CN113860900A (en) * | 2021-10-29 | 2021-12-31 | 西安美兰德新材料有限责任公司 | Rapid preparation method of high-performance carbon fiber composite material plate |
Non-Patent Citations (2)
| Title |
|---|
| 周长省: "《复合材料 第2版》", 哈尔滨工业大学出版社, pages: 173 - 198 * |
| 陈一哲: "汽车领域纤维复合材料构件轻量化设计与工艺研究进展", 《材料工程》, vol. 48, no. 12, pages 4 * |
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