CN115256927A - Carbon/carbon composite thermal insulation material prepared by 3D printing and preparation method thereof - Google Patents
Carbon/carbon composite thermal insulation material prepared by 3D printing and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/106—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
- B29C64/118—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using filamentary material being melted, e.g. fused deposition modelling [FDM]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/30—Auxiliary operations or equipment
- B29C64/379—Handling of additively manufactured objects, e.g. using robots
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/20—Post-treatment, e.g. curing, coating or polishing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29K2095/00—Use of bituminous materials as moulding material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2101/00—Use of unspecified macromolecular compounds as moulding material
- B29K2101/12—Thermoplastic materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
- B29K2105/0005—Condition, form or state of moulded material or of the material to be shaped containing compounding ingredients
- B29K2105/0038—Plasticisers
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Abstract
The present disclosure provides a method for preparing a carbon/carbon composite thermal insulation material by 3D printing, the method comprising: preparing a precursor wire; 3D printing and forming; pre-treating the mixture by fast burning; non-melting treatment; and performing high-temperature treatment to obtain the carbon/carbon composite heat-insulating material. The preparation method disclosed by the invention has the capability of preparing the special-shaped carbon/carbon composite thermal insulation material product, the structure of the distribution of material fibers and pores, which is related to the resin quantity and the resin uniformity degree, is more designable, and the carbon/carbon composite thermal insulation material product disclosed by the invention has more excellent structural performance and excellent thermal insulation capability because the fibers of the raw materials are combined with each other by adopting the melting capability of the fibers.
Description
Technical Field
The disclosure relates to the technical field of material forming, in particular to a carbon/carbon composite heat-insulating material prepared by 3D printing and a preparation method thereof.
Background
At present, carbon fiber hard felt used as a carbon/carbon composite thermal insulation material mainly adopts a forming process of carbon felt impregnation die pressing or soft carbon felt impregnation layered pasting. The impregnation die-pressing process has the defects of low interlayer strength of products, easy delamination and cracking of the products under the high-temperature use condition, short service life and the like, and is not convenient enough to disassemble and assemble due to relatively low strength; although the strength of the hard felt manufactured by adopting a layering sticking forming mode, namely graphite paper and carbon fiber are stuck at intervals is improved, the defects of increased heat conductivity coefficient, poor heat preservation performance and insufficient heat insulation effect of the product still exist. The fiber arrangement direction in the carbon/carbon composite thermal insulation material has a remarkable influence on the heat conductivity of the material, and when the heat flow is parallel to the fiber direction, the smaller the resistance of the heat flow is, the larger the heat conductivity coefficient is; and when the heat flow is vertical to the fiber direction, the larger the resistance is, the smaller the heat conductivity coefficient is. The needled felt hardened product is provided with longitudinally stretched carbon fiber tows, so that a part of carbon fibers are parallel to the heat flow direction, the heat conductivity coefficient is relatively large, and the energy consumption is large compared with that of a heat insulation material with a two-dimensional structure.
The pitch-based carbon fiber has the advantages of high carbon content, less volatilization, high purity, relatively small heat conductivity coefficient, high strength and no fracture, and even if the carbon fiber is fractured, the fracture surface formed by fracture is smooth and has little harm to the health of human bodies. The heat insulating material produced by using the asphalt-based carbon fiber has the advantages of excellent heat insulating performance, high carbon content, less volatile matter, less pollution, higher strength and the like.
Chinese patent CN104261853A relates to an asphalt-based carbon fiber non-woven felt heat-insulating cylinder and a manufacturing method thereof, and Chinese patent CN104230368A relates to an asphalt-based carbon fiber non-woven felt heat-insulating plate and a manufacturing method thereof.
Disclosure of Invention
In order to solve the above problems in the prior art, the present disclosure aims to provide a carbon/carbon composite thermal insulation material prepared by 3D printing, which is prepared by FDM technology, can be suitable for preparing a special-shaped thermal insulation material, has a strong designability of structure, and has an excellent thermal insulation performance, and a preparation method thereof.
In order to achieve the above purpose, the present disclosure adopts the following technical solutions:
the present disclosure provides a preparation method of a carbon/carbon composite thermal insulation material prepared by 3D printing, which comprises the following steps:
s1, preparing a precursor wire: mixing 60-80 parts by mass of spinning asphalt powder, 10-30 parts by mass of thermoplastic resin powder and 5-10 parts by mass of plasticizer to obtain precursor powder, and pressurizing, melting and extruding the precursor powder to prepare a precursor wire;
s2, 3D printing and forming: printing the precursor wire by utilizing fused deposition molding to obtain a carbon/carbon composite heat-insulating material prefabricated part;
s3, quick-firing pretreatment: embedding the carbon/carbon composite heat-insulating material prefabricated member by adopting ceramic particles, and heating to 150 to 180 ℃ for quick-burning pretreatment;
s4, non-melting treatment: performing infusible treatment on the carbon/carbon composite heat-insulating material prefabricated member which is subjected to quick-firing pretreatment and embedded by ceramic particles at the temperature of 180-250 ℃ under a negative pressure environment;
s5, high-temperature treatment: heating the carbon/carbon composite heat-insulating material prefabricated member which is subjected to non-melting treatment and embedded by ceramic particles to 1800-2200 ℃ in a nitrogen or argon atmosphere, preserving heat for 1-2 hours, performing high-temperature treatment, and removing the ceramic particles from the carbon/carbon composite heat-insulating material prefabricated member subjected to high-temperature treatment to obtain the carbon/carbon composite heat-insulating material.
In one possible embodiment, the melting temperature of the above spinning pitch powder is 150 ℃ or higher.
In one possible embodiment, the thermoplastic resin powder is polylactic acid or acrylonitrile-butadiene-styrene.
In one possible embodiment, the plasticizer is trioctyl trimellitate.
In a possible embodiment, the parameters for printing by fused deposition modeling include:
when the thermoplastic resin powder is polylactic acid, the printing temperature is 180/190/200/210 ℃; when the thermoplastic resin powder is acrylonitrile-butadiene-styrene, the printing temperature is 220/230/240/250 ℃;
the printing speed is 100/200/300/400 mm.min -1 ；
The printing precision is 0.1/0.2/0.3/0.4m of the layered thickness and 0.4/0.6/0.8/1.0mm of the scanning distance.
In one possible embodiment, the ceramic particles are silicon carbide particles with a particle size of 0.1 to 1mm.
In one possible embodiment, the condition of the quick-burning pretreatment is 0.1 to 1min.
In one possible embodiment, the non-melting condition is oxygen or air atmosphere, the flow rate is 2 to 10L/min, the pressure is 0.01 to 0.08MPa, and the non-melting time is 60 to 120min.
In one possible embodiment, the high-temperature treatment is performed under the condition of gradient temperature rise, wherein the temperature rise rate is 20 to 50 ℃/h to 900 ℃, the temperature is kept for 2h, then the temperature rise rate is 40 to 80 ℃/h to 1800 to 2200 ℃, and the temperature is kept for 1 to 2h; the flow of nitrogen or argon is 5 to 20L/min; the pressure is 0.08 to 0.1MPa.
The disclosure also provides a carbon/carbon composite thermal insulation material prepared by 3D printing, and the carbon/carbon composite thermal insulation material is prepared by any one of the preparation methods of the carbon/carbon composite thermal insulation material prepared by 3D printing.
The beneficial effect of the above-mentioned technical scheme that this disclosure provided includes at least:
firstly, spinning asphalt, thermoplastic resin and a plasticizer are fully mixed according to a certain proportion to obtain a thermoplastic carbon/carbon precursor which can be repeatedly heated, melted, cooled and solidified. Then, a precursor wire which can be used for fused deposition modeling is prepared by a pressurized melt extrusion modeling method. And then, preparing the carbon/carbon composite heat-insulating material prefabricated member with a complex structure by adopting an FDM (fused deposition modeling) technology. And finally, obtaining the carbon/carbon composite heat-insulating material through quick-firing pretreatment, infusible treatment and high-temperature treatment. The preparation method disclosed by the invention adopts the spinning pitch to prepare the carbon/carbon composite heat-insulating material, so that the step of preparing carbon fibers by adopting pitch is omitted, and the preparation process is simplified; the adopted thermoplastic resin has a pore-forming function in the preparation process, the preform is subjected to preliminary pore-forming through quick-firing pretreatment, and the preform is subjected to high-temperature treatment for pore-forming, so that the finally obtained carbon/carbon composite thermal insulation material has uniform pores, and the thermal insulation performance is further improved.
The thermoplastic carbon/carbon composite material precursor can be repeatedly heated, melted, cooled and solidified, is cracked in high-temperature treatment, and then realizes the preparation of 3D printing carbon/carbon composite heat-insulating materials with complex shapes by combining FDM with a cracking process, so that the intelligent quick forming effect is achieved, a common desktop FDM printer can realize the preparation of the carbon/carbon composite heat-insulating materials, and a new way of obtaining the carbon/carbon composite heat-insulating materials with quick forming, controllable structures and high appearance freedom design by fused deposition forming is developed. The preparation method disclosed by the invention has the capability of preparing the special-shaped carbon/carbon composite thermal insulation material product, the distribution of material fibers and pores is related to the amount of resin and the uniformity of the resin, the structure is more designable, and the fibers of the raw materials are combined with each other by adopting the melting capacity of the fibers, so that the carbon/carbon composite thermal insulation material product disclosed by the invention has more excellent structural performance.
Drawings
In order to more clearly explain the technical solutions in the embodiments of the present disclosure, the drawings that are needed to be used in the description of the embodiments will be briefly introduced below. Other features, objects, and advantages of the present application will become more apparent upon reading of the following detailed description of non-limiting embodiments thereof, with reference to the accompanying drawings.
Fig. 1 is a flowchart illustrating a method for preparing a carbon/carbon composite thermal insulation material by 3D printing according to an embodiment of the present disclosure;
fig. 2 (a) to fig. 2 (D) are schematic diagrams illustrating a micro-topography of a carbon/carbon composite thermal insulation material prepared by 3D printing according to an embodiment of the disclosure, wherein fig. 2 (a) is a schematic diagram illustrating a micro-topography of a longitudinal cross section of the carbon/carbon composite thermal insulation material prepared by 3D printing according to an embodiment of the disclosure under a scanning electron microscope with a magnification of 1000 times; fig. 2 (b) is an exemplary diagram of a cross-sectional micro-topography of a carbon/carbon composite thermal insulation material prepared by 3D printing under a scanning electron microscope with a magnification of 1000 times, provided by an embodiment of the present disclosure; fig. 2 (c) is an exemplary diagram of a longitudinal-section micro-topography of a carbon/carbon composite thermal insulation material prepared by 3D printing under a scanning electron microscope with a magnification of 500 times, provided by an embodiment of the present disclosure; fig. 2 (D) is an exemplary diagram of a cross-sectional micro-topography of a carbon/carbon composite thermal insulation material prepared by 3D printing under a scanning electron microscope with a magnification of 500 times according to an embodiment of the present disclosure.
Detailed Description
For a better understanding of the present application, the present disclosure is further illustrated by the following examples, and it is to be understood that these detailed descriptions are merely descriptive of exemplary embodiments of the present application and are not intended to limit the scope of the present application in any way. The expression "and/or" includes any and all combinations of one or more of the associated listed items.
The present disclosure is described in further detail below:
as shown in fig. 1, the present disclosure provides a method for preparing a carbon/carbon composite thermal insulation material by 3D printing, comprising the steps of:
s1, preparing a precursor wire: mixing 60-80 parts by mass of spinning asphalt powder, 10-30 parts by mass of thermoplastic resin powder and 5-10 parts by mass of plasticizer to obtain precursor powder, and pressurizing, melting and extruding the precursor powder to prepare a precursor wire. Wherein, the melting temperature of one of the raw materials used is 150 ℃ or higher, the spinning asphalt powder can be petroleum spinning asphalt powder or coal spinning asphalt powder, the thermoplastic resin powder is polylactic acid or acrylonitrile-butadiene-styrene, and the plasticizer is trioctyl trimellitate.
By way of example, the above raw material powders are mixed by a ball mill for 28 to 48h to obtain a mixed precursor powder, and the obtained precursor powder is a thermoplastic carbon/carbon precursor powder.
Specifically, the melting temperature in the process of preparing the precursor wire by pressurizing, melting and extruding the precursor powder can be 150 to 220 ℃, and the diameter of the precursor wire is 1.0 to 3.0mm.
S2, 3D printing and forming: and printing the precursor wire according to a preset size and structural design by utilizing Fused Deposition Modeling (FDM) technology to obtain the carbon/carbon composite heat-insulating material prefabricated part.
Specifically, the parameters for printing by fused deposition modeling include: when the thermoplastic resin powder is polylactic acid, the printing temperature is 180/190/200/210 ℃; when the thermoplastic resin powder is acrylonitrile-butadiene-styrene, the printing temperature is 220/230/240/250 ℃; the printing speed is 100/200/300/400 mm.min < -1 >; the printing precision is 0.1/0.2/0.3/0.4m of the layered thickness and 0.4/0.6/0.8/1.0mm of the scanning interval.
S3, quick-firing pretreatment: embedding the carbon/carbon composite heat insulation material prefabricated member by using ceramic particles, and heating to 150-180 ℃ for quick-burning pretreatment. Wherein the ceramic particles are silicon carbide particles with the particle size of 0.1-1mm.
Specifically, the condition of the quick-burning pretreatment is that the treatment time is 0.1 to 1min.
S4, non-melting treatment: the carbon/carbon composite heat-insulating material prefabricated member which is subjected to quick-firing pretreatment and embedded by ceramic particles is subjected to infusible treatment at the temperature of 180-250 ℃ in a negative pressure environment.
Specifically, the non-melting treatment condition is oxygen or air atmosphere, the flow rate is 2 to 10L/min, the pressure is 0.01 to 0.08MPa, and the non-melting treatment time is 60 to 120min.
S5, high-temperature treatment: heating the carbon/carbon composite heat-insulating material prefabricated member which is subjected to non-melting treatment and is embedded by ceramic particles to 1800 to 2200 ℃ in a nitrogen or argon atmosphere, carrying out heat preservation for 1 to 2 hours, carrying out high-temperature treatment, and removing the ceramic particles from the carbon/carbon composite heat-insulating material prefabricated member subjected to high-temperature treatment to obtain the carbon/carbon composite heat-insulating material.
Specifically, the high-temperature treatment condition is gradient temperature rise, the temperature is raised to 900 ℃ at the temperature rise rate of 20 to 50 ℃/h, the temperature is kept for 2h, then the temperature is raised to 1800 to 2200 ℃ at the temperature rise rate of 40 to 80 ℃/h, and the temperature is kept for 1 to 2h; the flow of nitrogen or argon is 5 to 20L/min; the pressure is 0.08 to 0.1MPa.
The disclosure also provides a carbon/carbon composite thermal insulation material prepared by 3D printing, which is prepared by the preparation method of any one of the carbon/carbon composite thermal insulation materials prepared by 3D printing. As an example, the microscopic morphology of the carbon/carbon composite thermal insulation material of the present disclosure observed by an electron microscope can be as shown in fig. 2 (a) -2 (d), and it can be found that the precursor of the carbon/carbon composite thermal insulation material shrinks uniformly, forming the carbon/carbon composite thermal insulation material with a porous skeleton.
The beneficial effect of the above-mentioned technical scheme that this disclosure provided includes at least:
firstly, spinning asphalt, thermoplastic resin and a plasticizer are fully mixed according to a certain proportion to obtain a thermoplastic carbon/carbon precursor which can be repeatedly heated, melted, cooled and solidified. Then, a precursor wire which can be used for fused deposition modeling is prepared by a pressurized melt extrusion modeling method. And then, preparing the carbon/carbon composite heat-insulating material prefabricated member with a complex structure by adopting an FDM (fused deposition modeling) technology. And finally, obtaining the carbon/carbon composite heat-insulating material through quick-firing pretreatment, infusible treatment and high-temperature treatment. The preparation method disclosed by the invention adopts the spinning asphalt to prepare the carbon/carbon composite heat-insulating material, so that the step of preparing carbon fibers by adopting the asphalt is omitted, and the preparation process is simplified; the thermoplastic resin adopted in the preparation process can be dissipated at a higher temperature, the pore-forming function is realized, the pore-forming is performed preliminarily in the prefabricated part through the fast-firing pretreatment, the pore-forming is performed through the high-temperature treatment, and the finally obtained carbon/carbon composite thermal insulation material has uniform pores, so that the thermal insulation performance is further improved.
The thermoplastic carbon/carbon composite material precursor can be repeatedly heated, melted, cooled and solidified, is cracked in high-temperature treatment, and then realizes the preparation of 3D printing carbon/carbon composite heat-insulating materials with complex shapes by combining FDM with a cracking process, so that the intelligent quick forming effect is achieved, a common desktop FDM printer can realize the preparation of the carbon/carbon composite heat-insulating materials, and a new way of obtaining the carbon/carbon composite heat-insulating materials with quick forming, controllable structures and high appearance freedom design by fused deposition forming is developed. The preparation method disclosed by the invention has the capability of preparing the special-shaped carbon/carbon composite thermal insulation material product, the material fiber and pore distribution in the prepared carbon/carbon composite thermal insulation material are related to the resin amount and the resin uniformity, the structure has greater designability, and the fiber melting capability of the fiber is adopted to realize the mutual combination of the fibers of the raw materials, so that the carbon/carbon composite thermal insulation material product disclosed by the invention has more excellent structural performance.
The technical solution of the present application will be further described in detail with reference to the following examples.
Example 1
60 parts by mass of petroleum spinning asphalt powder, 30 parts by mass of polylactic acid powder and 10 parts by mass of trioctyl trimellitate powder are weighed, and the sum of the parts by mass of all the raw materials is 100 parts. Mixing all the raw materials, adding a little alcohol, putting the mixture into a ball mill for mixing for 28 hours, taking out the mixture after ball milling, and carrying out vacuum drying at the temperature of 60 ℃ to obtain precursor powder. The precursor powder was melted under pressure at 150 ℃ using an extruder to prepare a thermoplastic precursor wire having a diameter of about 1mm, which was used for fused deposition modeling. And printing the precursor wire into a carbon/carbon composite heat-insulating material prefabricated part with a preset shape by using an FDM machine under the printing parameters shown in the following table.
Table 1 example 1 printing parameters
The carbon/carbon composite heat-insulating material prefabricated member is embedded by using silicon carbide particles with the particle size of 0.1mm, and is quickly placed at the temperature ofIn an oven at 150 ℃, the retention time is 1min, so that the fibers of the carbon/carbon composite heat-insulating material prefabricated member can be mutually adhered due to surface melting. And (3) placing the carbon/carbon composite heat-insulating material prefabricated part subjected to the quick-firing pretreatment and silicon carbide particles for embedding into a non-melting furnace, introducing oxygen with the flow rate of 2L/min, vacuumizing to 0.01MPa, heating to 180 ℃, and performing non-melting treatment for 60min. Placing the carbon/carbon composite heat-insulating material prefabricated member subjected to non-melting treatment and silicon carbide particles for embedding into a high-temperature furnace, and introducing nitrogen (N) with gas flow of 5L/min 2 ) Under the atmosphere, the pressure in the furnace is set to be 0.08MPa, the temperature is increased to 900 ℃ at the heating rate of 20 ℃/h, and the temperature is kept for 2h; and continuously heating to 1800 ℃ at the heating rate of 40 ℃/h, and preserving heat for 1h to finish high-temperature treatment to obtain the carbon/carbon composite heat-insulating material product.
Example 2
80 parts by weight of coal-based spinning asphalt powder, 15 parts by weight of acrylonitrile-butadiene-styrene powder and 5 parts by weight of trioctyl trimellitate powder are weighed, and the sum of the parts by weight of all the raw materials is 100 parts. Mixing all the raw materials, adding a little alcohol, putting the mixture into a ball mill, mixing for 48 hours, taking out the mixture after ball milling, and carrying out vacuum drying at 60 ℃ to obtain precursor powder. The precursor powder was melted under pressure at 220 ℃ using an extruder to prepare a thermoplastic precursor wire having a diameter of about 3mm, which was used for fused deposition modeling. And printing the precursor wire into a carbon/carbon composite heat-insulating material prefabricated part with a preset shape by using an FDM machine under the printing parameters shown in the following table.
Table 2 example 2 printing parameters
The carbon/carbon composite heat-insulating material prefabricated part is embedded by using silicon carbide particles with the particle size of 1mm, and is quickly placed in an oven with the temperature of 180 ℃ for 0.5min, so that fibers of the carbon/carbon composite heat-insulating material prefabricated part can be adhered to each other due to surface melting. And (3) placing the carbon/carbon composite heat-insulating material prefabricated part subjected to the quick-firing pretreatment and silicon carbide particles for embedding into a non-melting furnace, introducing air with the flow rate of 10L/min, vacuumizing to 0.08MPa, heating to 250 ℃, and performing non-melting treatment for 120min. Placing the carbon/carbon composite heat-insulating material prefabricated part subjected to non-melting treatment and silicon carbide particles for embedding into a high-temperature furnace, setting the pressure in the furnace to be 0.1MPa under the argon (Ar) atmosphere with the gas flow of 20L/min, heating to 900 ℃ at the heating rate of 50 ℃/h, and preserving heat for 2h; and continuously heating to 2200 ℃ at the heating rate of 80 ℃/h, and preserving the heat for 2h to finish high-temperature treatment to obtain the carbon/carbon composite heat-insulating material product.
Example 3
80 parts by mass of coal-based spinning asphalt powder, 10 parts by mass of acrylonitrile-butadiene-styrene powder and 10 parts by mass of trioctyl trimellitate powder are weighed, and the sum of the parts by mass of all the raw materials is 100 parts. Mixing all the raw materials, adding a little alcohol, putting the mixture into a ball mill for mixing for 38 hours, taking out the mixture after ball milling, and carrying out vacuum drying at the temperature of 60 ℃ to obtain precursor powder. The precursor powder was melted under pressure at 185 ℃ using an extruder to prepare a thermoplastic precursor wire having a diameter of about 2mm, which was used for fused deposition modeling. And printing the precursor wire into a carbon/carbon composite heat-insulating material prefabricated part with a preset shape by using an FDM machine under the printing parameters shown in the following table.
Table 3 example 3 printing parameters
The carbon/carbon composite heat-insulating material prefabricated part is embedded by using silicon carbide particles with the particle size of 0.5mm, and is quickly placed in an oven with the temperature of 165 ℃ for 0.1min, so that fibers of the carbon/carbon composite heat-insulating material prefabricated part can be mutually adhered due to surface melting. And (3) placing the carbon/carbon composite heat-insulating material prefabricated part subjected to the quick-firing pretreatment and silicon carbide particles for embedding into a non-melting furnace, introducing air with the flow rate of 6L/min, vacuumizing to 0.04MPa, heating to 215 ℃, and performing non-melting treatment for 90min. Placing the carbon/carbon composite heat-insulating material prefabricated part subjected to non-melting treatment and silicon carbide particles for embedding into a high-temperature furnace, setting the pressure in the furnace to be 0.09MPa under the argon (Ar) atmosphere with the gas flow of 12L/min, heating to 900 ℃ at the heating rate of 35 ℃/h, and preserving heat for 2h; and continuously heating to 2200 ℃ at the heating rate of 60 ℃/h, and preserving the heat for 1.5h to finish high-temperature treatment to obtain the carbon/carbon composite heat-insulating material product.
While particular embodiments of the present disclosure have been described in the foregoing specification, the various illustrations do not limit the spirit of the disclosure, and one of ordinary skill in the art, after reading the description, can make modifications and alterations to the particular embodiments described above without departing from the spirit and scope of the disclosure.
Claims (10)
1. The preparation method of the carbon/carbon composite heat-insulating material prepared by 3D printing is characterized by comprising the following steps of:
s1, preparing a precursor wire: mixing 60-80 parts by mass of spinning asphalt powder, 10-30 parts by mass of thermoplastic resin powder and 5-10 parts by mass of plasticizer to obtain precursor powder, and pressurizing, melting and extruding the precursor powder to prepare a precursor wire;
s2, 3D printing and forming: printing the precursor wire by utilizing fused deposition molding to obtain a carbon/carbon composite heat-insulating material prefabricated part;
s3, quick-firing pretreatment: embedding the carbon/carbon composite heat-insulating material prefabricated member by adopting ceramic particles, and heating to 150-180 ℃ for quick-burning pretreatment;
s4, non-melting treatment: carrying out infusible treatment on the carbon/carbon composite heat-insulating material prefabricated member which is subjected to fast firing pretreatment and embedded by ceramic particles at the temperature of 180-250 ℃ in a negative pressure environment;
s5, high-temperature treatment: heating the carbon/carbon composite heat-insulating material prefabricated member which is subjected to non-melting treatment and embedded by ceramic particles to 1800-2200 ℃ in a nitrogen or argon atmosphere, preserving heat for 1-2 hours, performing high-temperature treatment, and removing the ceramic particles from the carbon/carbon composite heat-insulating material prefabricated member subjected to high-temperature treatment to obtain the carbon/carbon composite heat-insulating material.
2. The method for preparing carbon/carbon composite thermal insulation material by 3D printing as claimed in claim 1, wherein the melting temperature of the spinning pitch powder is 150 ℃ or higher.
3. The method for preparing the carbon/carbon composite thermal insulation material prepared by 3D printing according to claim 1, wherein the thermoplastic resin powder is polylactic acid or acrylonitrile-butadiene-styrene.
4. The method for preparing the carbon/carbon composite thermal insulation material prepared by 3D printing according to claim 1, wherein the plasticizer is trioctyl trimellitate.
5. The method for preparing carbon/carbon composite thermal insulation material by 3D printing according to claim 3, wherein the parameters for printing by fused deposition modeling comprise:
when the thermoplastic resin powder is polylactic acid, the printing temperature is 180/190/200/210 ℃; when the thermoplastic resin powder is acrylonitrile-butadiene-styrene, the printing temperature is 220/230/240/250 ℃;
the printing speed is 100/200/300/400 mm.min -1 ；
The printing precision is 0.1/0.2/0.3/0.4m of the layered thickness and 0.4/0.6/0.8/1.0mm of the scanning distance.
6. The method for preparing the carbon/carbon composite thermal insulation material prepared by 3D printing according to claim 1, wherein the ceramic particles are silicon carbide particles with the particle size of 0.1-1mm.
7. The method for preparing the carbon/carbon composite thermal insulation material prepared by 3D printing according to claim 1, wherein the condition of the quick firing pretreatment is 0.1-1min.
8. The method for preparing the carbon/carbon composite thermal insulation material prepared by 3D printing according to claim 1, wherein the non-melting treatment condition is an oxygen or air atmosphere, the flow rate is 2-10L/min, the pressure is 0.01-0.08MPa, and the non-melting treatment time is 60-120min.
9. The method for preparing the carbon/carbon composite thermal insulation material prepared by 3D printing according to claim 1, wherein the high-temperature treatment condition is gradient temperature rise, the temperature is raised to 900 ℃ at a temperature rise rate of 20 to 50 ℃/h, the temperature is kept for 2h, then the temperature is raised to 1800 to 2200 ℃ at a temperature rise rate of 40 to 80 ℃/h, and the temperature is kept for 1 to 2h; the flow rate of nitrogen or argon is 5 to 20L/min; the pressure is 0.08 to 0.1MPa.
10. The carbon/carbon composite thermal insulation material prepared by 3D printing is characterized by being prepared by the preparation method of the carbon/carbon composite thermal insulation material prepared by 3D printing according to any one of claims 1 to 9.
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