CN115806440A - Embedded direct-writing 3D printing preparation method of steel fiber ceramic composite material - Google Patents

Embedded direct-writing 3D printing preparation method of steel fiber ceramic composite material Download PDF

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CN115806440A
CN115806440A CN202211397118.3A CN202211397118A CN115806440A CN 115806440 A CN115806440 A CN 115806440A CN 202211397118 A CN202211397118 A CN 202211397118A CN 115806440 A CN115806440 A CN 115806440A
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steel fiber
writing
composite material
ceramic composite
printing
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CN115806440B (en
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涂勇强
吴志聪
何凯伦
黄奇家
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Fujian Xinghai Communication Technology Co Ltd
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Fujian Xinghai Communication Technology Co Ltd
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Priority to CN202311340890.6A priority patent/CN117623791A/en
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Abstract

The invention relates to the technical field of preparation of steel fiber ceramic composite materials, in particular to an embedded direct-writing 3D printing preparation method of a steel fiber ceramic composite material, which comprises the following steps: s1, preparing ceramic matrix suspension and steel fiber ink; s2, performing embedded direct-writing 3D printing; and S3, drying, degreasing and sintering the printed part. The method has the advantages of low cost, high speed, simple processing, no need of clean room environment, high precision of the prepared steel fiber ceramic composite material and good practicability.

Description

Embedded direct-writing 3D printing preparation method of steel fiber ceramic composite material
Technical Field
The invention relates to the technical field of preparation of steel fiber ceramic composite materials, in particular to an embedded direct-writing 3D printing preparation method of a steel fiber ceramic composite material.
Background
Ceramic materials have the advantages of high strength, high hardness, good thermal stability and oxidation resistance, making them the material of choice for applications involving exposure to harsh environments. However, ceramic materials have the disadvantages of low fracture energy and brittleness. In order to improve the fracture energy of ceramic materials, a common way at present is to fill steel fiber fillers in ceramic matrix to prepare steel fiber ceramic composite materials.
However, in the existing preparation method of the steel fiber ceramic composite material, the steel fibers and the ceramic slurry are directly mixed, for example, the application number is 202110862623.X, and the Chinese patent application named as a non-fired high-strength metal ceramic composite material, the preparation method and the application thereof cannot design the orientation of the steel fibers, so that the steel fiber structure cannot be designed to improve the fracture energy of the composite material by optimizing the design of the steel fiber structure, and the potential of the steel fiber ceramic composite material is restricted.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the embedded direct-writing 3D printing preparation method of the steel fiber ceramic composite material is low in cost and high in precision.
In order to solve the technical problems, the invention adopts the technical scheme that: an embedded direct-writing 3D printing preparation method of a steel fiber ceramic composite material comprises the following steps:
s1, preparing ceramic matrix suspension and steel fiber ink;
s2, performing embedded direct-writing 3D printing;
and S3, drying, degreasing and sintering the printed part.
Further, the step S1 specifically includes the step S11:
dissolving temperature-sensitive hydrogel powder and distilled water in the distilled water according to the mass percent of 25wt% and 30wt% respectively, and storing the solution in an environment at 0-4 ℃ for 24-36 hours to obtain two parts of Pluronic gel with the mass percent of 25wt% and 30wt% respectively.
Further, the step S1 specifically includes a step S12:
mixing alumina powder and Pluronic gel with the mass percent of 25wt% according to the weight ratio of 7:3, adding a dispersant with the mass of 1-3% of the mass of the alumina powder to obtain a mixture, and placing the mixture in an ice bath for cooling for 20-30 minutes.
Further, the step S1 specifically includes a step S13:
and stirring the cooled mixture at the speed of 2000-2500 rpm for 5-10 minutes, then placing the mixture in an ice bath for cooling for 20-30 minutes, and repeatedly stirring and cooling for 3-5 times to obtain the ceramic matrix suspension.
Further, the step S1 specifically includes a step S14:
mixing steel powder and 30wt% of Pluronic gel according to the volume ratio of 1:3, adding 0.5-1.5 wt% of dispersant by weight of the steel powder to obtain a mixture, and placing the mixture in an ice bath for cooling for 20-30 minutes.
Further, the step S1 specifically includes the step S15:
and stirring the cooled mixture for 5-10 minutes at a speed of 2000-2500 rpm, then placing the mixture in an ice bath for cooling for 20-30 minutes, and repeating stirring and cooling for 3-5 times to obtain the steel fiber ink.
Further, the step S2 specifically includes the step S21:
and respectively placing the ceramic matrix suspension and the steel fiber ink in a vacuum environment for drying for 60-70 minutes.
Further, the step S2 specifically includes the step S22:
and cooling the dried ceramic matrix suspension to 0-10 ℃, and pouring into a silica gel mold coated with silicone oil.
Further, the step S2 specifically includes the step S23:
and (3) placing the silica gel mold in a water bath with the temperature of 15-20 ℃, injecting the steel fiber ink into a needle cylinder for direct-writing 3D printing, and extruding ink filaments with the diameter of 10-700 um by using a nozzle with the inner diameter of 10-600 um.
Further, the S3 specifically includes the steps of:
s31, taking down the silica gel mold containing the ceramic substrate suspension and the printed ink, and drying the silica gel mold in an environment with the temperature of 32 ℃ for 1 to 2 weeks;
s32, taking the dried ceramic matrix suspension out of the silica gel mold, placing the ceramic matrix suspension in a sintering furnace, heating the ceramic matrix suspension from room temperature to 350 ℃ at a heating rate of 1 ℃/min, keeping the temperature for 1-2 hours, then continuously heating the ceramic matrix suspension to 500 ℃ at a heating rate of 2 ℃/min, keeping the temperature for 2-3 hours, and then opening a box to cool the ceramic matrix suspension to the normal temperature;
and S33, heating the temperature from room temperature to 1550 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 2-3 hours, and finally opening the box and cooling to the normal temperature.
The invention has the beneficial effects that: the invention overcomes the problems that the existing preparation method of the steel fiber ceramic composite material directly mixes the steel fiber and the ceramic slurry, and the orientation of the steel fiber can not be designed, so that the steel fiber structure can not be designed to improve the fracture energy of the composite material by optimizing the steel fiber structure design, and the potential of the steel fiber ceramic composite material is restricted. The method is based on an embedded direct-writing 3D printing technology, and is characterized in that a ceramic gel with a self-repairing function is prepared, the gel can enable a direct-writing 3D printing nozzle to move in the ceramic gel, the nozzle can heal without defect after passing through the ceramic gel, meanwhile, the direct-writing 3D printing is used for printing steel fiber ink in the ceramic gel, the gel can form compact and flawless ceramic in subsequent heat treatment, the steel fiber ink is wrapped, and finally, the steel fiber ink and the ceramic gel are solidified through sintering to prepare the steel fiber ceramic composite material with a designable steel fiber structure. The method has the advantages of low cost, high speed, simple processing, no need of clean room environment, high precision of the prepared steel fiber ceramic composite material and good practicability.
Drawings
FIG. 1 is a schematic flow chart of an embedded direct-writing 3D printing preparation method of a steel fiber ceramic composite material according to the present invention;
fig. 2 is a schematic diagram of a printer setting for performing embedded direct-write 3D printing in step S2 according to an embodiment of the present invention;
fig. 3 is a schematic diagram illustrating extrusion of steel fiber ink for embedded direct-write 3D printing in step S2 according to an embodiment of the present invention;
description of the reference symbols:
1. a piston; 2. a needle cylinder; 3. a nozzle; 4. a silica gel mold; 5. water bath; 6. a ceramic matrix suspension; 7. steel fiber ink.
Detailed Description
In order to explain technical contents, achieved objects, and effects of the present invention in detail, the following description is made with reference to the accompanying drawings in combination with the embodiments.
The direct-writing 3D printing belongs to an extrusion type 3D printing technology in an additive manufacturing technology, has a wide application prospect in the preparation of ceramic materials, and is used for preparing a ceramic blank body by continuously extruding ceramic slurry, and then drying, degreasing and sintering the ceramic blank body to finally prepare a compact ceramic part. Embedded direct-write 3D printing is an emerging variant of direct-write 3D printing, which is based on printing complex structures in a soft support matrix, with excellent manufacturing freedom, and can produce complex micro-scale structures. Therefore, the invention provides a method for preparing a steel fiber ceramic composite material by using embedded direct-writing 3D printing, so that a complex designable steel fiber structure can be printed in compact ceramics.
Referring to fig. 1 to 3, an embedded direct-writing 3D printing preparation method of a steel fiber ceramic composite material includes the following steps:
s1, preparing a ceramic matrix suspension 6 and steel fiber ink 7;
s2, performing embedded direct-writing 3D printing;
and S3, drying, degreasing and sintering the printed parts.
As can be seen from the above description, the beneficial effects of the present invention are: the invention overcomes the problem that the existing preparation method of the steel fiber ceramic composite material directly mixes the steel fiber with the ceramic slurry, and the orientation of the steel fiber can not be designed, so that the steel fiber structure can not be designed to improve the fracture energy of the composite material by optimizing the design of the steel fiber structure, and the potential of the steel fiber ceramic composite material is restricted. The method is based on an embedded direct-writing 3D printing technology, and is characterized in that a ceramic gel with a self-repairing function is prepared, the gel can enable a direct-writing 3D printing nozzle to move in the ceramic gel, the nozzle can heal without defect after passing through the ceramic gel, meanwhile, the direct-writing 3D printing is used for printing steel fiber ink in the ceramic gel, the gel can form compact and flawless ceramic in subsequent heat treatment, the steel fiber ink is wrapped, and finally, the steel fiber ink and the ceramic gel are solidified through sintering to prepare the steel fiber ceramic composite material with a designable steel fiber structure. The method has the advantages of low cost, high speed, simple processing, no need of clean room environment, high precision of the prepared steel fiber ceramic composite material and good practicability.
In an optional embodiment, the S1 specifically includes step S11:
dissolving the temperature-sensitive hydrogel powder and distilled water in the distilled water according to the mass percent of 25wt% and 30wt% respectively, and storing the solution in an environment at 0-4 ℃ for 24-36 hours to obtain two parts of Pluronic gel with the mass percent of 25wt% and 30wt% respectively.
As can be seen from the above description, pluronic is a temperature-sensitive hydrogel composed of poly (ethylene oxide) -poly (propylene oxide) -poly (ethylene oxide) (PEO-PPO-PEO). Pluronic powder and distilled water were dissolved in distilled water at 25wt% and 30wt%, respectively, and stored in a refrigerator at 0-4 ℃ for 24-36 hours to obtain two Pluronic gels at 25wt% and 30wt%, respectively.
Preferably, the Pluronic powder is of the brand: pluronic F127.
In an optional embodiment, the S1 specifically includes step S12:
mixing alumina powder and Pluronic gel with the mass percent of 25wt% according to the weight ratio of 7:3, adding a dispersant with the mass of 1-3% of the mass of the alumina powder to obtain a mixture, and placing the mixture in an ice bath for cooling for 20-30 minutes.
In an optional embodiment, the S1 specifically includes step S13:
and stirring the cooled mixture for 5-10 minutes at a speed of 2000-2500 rpm, then placing the mixture in an ice bath for cooling for 20-30 minutes, and repeatedly stirring and cooling for 3-5 times to obtain a ceramic matrix suspension 6.
As can be seen from the above description, alumina powder is added to Pluronic gel with a mass percentage of 25wt% in a weight ratio of 7 to 3, a dispersant is added in an amount of 1 to 3% by mass of the alumina powder, the mixture is cooled in an ice bath for 20 to 30 minutes, the cooled mixture is stirred in a stirrer at a speed of 2000 rpm to 2500 rpm for 5 to 10 minutes, then subsequently cooled in an ice bath for 20 to 30 minutes, and the mixing and cooling steps are repeated 3 to 5 times to obtain a ceramic matrix suspension 6;
preferably, the dispersant is of the brand number: dolapix CA.
Preferably, the mixing and cooling steps are performed multiple times in order to mix the powders sufficiently to obtain a homogeneous, lump-free ceramic matrix suspension 6.
In an optional embodiment, the S1 specifically includes step S14:
mixing steel powder and 30wt% of Pluronic gel according to the volume ratio of 1:3, adding 0.5-1.5 wt% of dispersant by weight of the steel powder to obtain a mixture, and placing the mixture in an ice bath for cooling for 20-30 minutes.
In an optional embodiment, the step S1 specifically includes the step S15:
and stirring the cooled mixture at the speed of 2000-2500 rpm for 5-10 minutes, then placing the mixture in an ice bath for cooling for 20-30 minutes, and repeating stirring and cooling for 3-5 times to obtain the steel fiber ink 7.
From the above description, the steel powder is mixed with Pluronic gel prepared in step S101 in a mass percentage of 30wt% in a volume ratio of 1
Preferably, the steel powder has a particle size of 5 to 8um.
Preferably, the dispersant is of the brand number: dolapix CA.
Preferably, the purpose of performing the mixing and cooling steps multiple times is to mix the powder sufficiently to obtain a homogeneous steel fibre ink 7.
In an optional embodiment, the step S2 specifically includes the step S21:
and respectively placing the ceramic matrix suspension 6 and the steel fiber ink 7 in a vacuum environment for drying for 60-70 minutes.
As can be seen from the above description, the above steps are used to eliminate air bubbles in the ceramic matrix suspension 6 and the steel fiber ink 7.
In an optional embodiment, the step S2 specifically includes the step S22:
and cooling the dried ceramic matrix suspension 6 to 0-10 ℃, and pouring the ceramic matrix suspension into a silica gel mold 4 coated with silicone oil.
As can be seen from the above description, the purpose of cooling the ceramic matrix suspension 6 to 0-10 c is that the viscosity of the ceramic matrix suspension 6 is low at 0-10 c, facilitating filling of the silica gel mold 4.
Preferably, the silicone mold 4 is a rectangular container with an upper opening, and the material is silicone.
Preferably, the silicone oil is coated inside the silicone mold 4 for the purpose of facilitating mold release.
In an optional embodiment, a three-dimensional model of a flow channel to be printed is built in three-dimensional modeling software, the three-dimensional model is additionally stored as an STL file and is imported into slicing software, printing parameters are set in the slicing software, a G-code file is generated, and the G-code file is imported into a direct-writing 3D printer for embedded direct-writing 3D printing.
In an optional embodiment, the S2 specifically includes step S23:
the silica gel mold 4 is placed in a water bath 5 with the temperature of 15-20 ℃, the steel fiber ink 7 is injected into a needle cylinder 2 for direct-writing 3D printing, a piston 1 is arranged on the needle cylinder 2, and an ink filament with the diameter of 10-700 um is extruded by a nozzle 3 with the inner diameter of 10-600 um.
As can be seen from the above description, the silicone mold 4 is placed in a water bath 5 at a temperature of 15-20 ℃ during printing to ensure that the ceramic matrix suspension 6 in the silicone mold 4 has a temperature of 15-20 ℃ during printing in order to allow the ceramic matrix suspension 6 to have sufficient viscosity to support the printed ink.
Preferably, during printing, the nozzle 3 is in a ceramic matrix suspension 6 and the ink is extruded as filaments suspended in the ceramic matrix suspension 6.
In an optional embodiment, the S3 specifically includes the steps of:
s31, drying: taking down the silica gel mold 4 containing the ceramic substrate suspension 6 and the printed ink, and drying in an environment with the temperature of 32 ℃ for 1-2 weeks;
s32, degreasing: taking the dried ceramic matrix suspension 6 out of the silica gel mold 4, placing the ceramic matrix suspension in a sintering furnace, heating the ceramic matrix suspension from room temperature to 350 ℃ at a heating rate of 1 ℃/min, keeping the temperature for 1-2 hours, then continuously heating the ceramic matrix suspension to 500 ℃ at a heating rate of 2 ℃/min, keeping the temperature for 2-3 hours, and then opening the box to cool the ceramic matrix suspension to the normal temperature;
s33, sintering: heating the temperature from room temperature to 1550 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 2-3 hours, and finally opening the box and cooling to the normal temperature.
From the above description, it can be seen that the ceramic matrix suspension becomes a dense ceramic part by drying, degreasing and sintering, and the steel fiber ink is cured during sintering, and finally a high-precision designable complex steel fiber structure is formed in the ceramic part, thereby completing the preparation of the steel fiber ceramic composite material.
Referring to fig. 1 to 3, a first embodiment of the present invention is: an embedded direct-writing 3D printing preparation method of a steel fiber ceramic composite material comprises the following steps:
s1, preparing a ceramic matrix suspension 6 and steel fiber ink 7;
s2, performing embedded direct-writing 3D printing;
and S3, drying, degreasing and sintering the printed part.
Further, the specific operation of step S1 is:
s101, dissolving Pluronic (temperature-sensitive hydrogel composed of poly (ethylene oxide) -poly (propylene oxide) -poly (ethylene oxide) (PEO-PPO-PEO)) powder and distilled water in the distilled water according to the mass percent of 25wt% and 30wt% respectively, and storing the solution in a refrigerator at 0-4 ℃ for 24-36 hours to obtain two Pluronic gels with the mass percent of 25wt% and 30wt% respectively;
s102, adding aluminum oxide powder into Pluronic gel which is prepared in the step S101 and has the mass percent of 25wt% in a weight ratio of 7;
s103, mixing steel powder with Pluronic gel which is prepared in the step S101 and accounts for 30wt% in percentage by mass according to a volume ratio of 1;
the specific operation of step S2 is:
s201, respectively putting the ceramic matrix suspension 6 prepared in the step S102 and the steel fiber ink 7 prepared in the step S103 into a vacuum drier for drying for 60-70 minutes, and eliminating bubbles in the ceramic matrix suspension 6 and the steel fiber ink 7;
s202, cooling the ceramic matrix suspension 6 obtained in the step 201 to 0-10 ℃, and pouring the ceramic matrix suspension into a silicone mold 4 coated with silicone oil;
s203, injecting the steel fiber ink 7 obtained in the step 201 into the needle cylinder 2 for direct-writing 3D printing;
s204, constructing a three-dimensional model of the flow channel to be printed in three-dimensional modeling software, storing the three-dimensional model as an STL file, importing the STL file into slicing software, setting printing parameters in the slicing software, generating a G-code file, and importing the G-code file into a direct-writing 3D printer for embedded direct-writing 3D printing;
the specific operation of step S3 is:
s301, drying: after printing is finished, taking down the silica gel mold 4 containing the ceramic matrix suspension 6 and the printed ink, putting the silica gel mold into a convection oven, setting the humidity in the oven to be 72 +/-3% by placing supersaturated sodium chloride solution in the oven, setting the temperature of the oven to be 32 ℃, and placing a fan in the oven to promote air circulation, wherein the drying time is 1-2 weeks;
s302, degreasing: taking out the ceramic substrate suspension 6 dried in the step S301 from the silica gel mold 4, placing the ceramic substrate suspension in a sintering furnace, and in order to ensure that the part does not crack in the sintering process, degreasing the part before sintering, wherein the specific operations are as follows: heating up to 350 ℃ from room temperature at a heating rate of 1 ℃/min, keeping the temperature for 1-2 hours, continuously heating up to 500 ℃ at a heating rate of 2 ℃/min, keeping the temperature for 2-3 hours after the temperature reaches 500 ℃, and opening the box to cool to normal temperature;
s303, sintering: sintering after degreasing, which comprises the following specific operations: heating the temperature from room temperature to 1550 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 2-3 hours after the temperature reaches 1550 ℃, and opening the box to cool to the normal temperature.
In conclusion, the invention overcomes the problems that the existing preparation method of the steel fiber ceramic composite material directly mixes the steel fibers and the ceramic slurry, and the orientation of the steel fibers can not be designed, so that the steel fiber structure can not be designed to improve the fracture energy of the composite material by optimizing the steel fiber structure design, and the potential of the steel fiber ceramic composite material is restricted. The method is based on an embedded direct-writing 3D printing technology, and is characterized in that a ceramic gel with a self-repairing function is prepared, the gel can enable a direct-writing 3D printing nozzle to move in the ceramic gel, the nozzle can heal without defect after passing through the ceramic gel, meanwhile, the direct-writing 3D printing is used for printing steel fiber ink in the ceramic gel, the gel can form compact and flawless ceramic in subsequent heat treatment, the steel fiber ink is wrapped, and finally, the steel fiber ink and the ceramic gel are solidified through sintering to prepare the steel fiber ceramic composite material with a designable steel fiber structure. The method has the advantages of low cost, high speed, simple processing, no need of clean room environment, high precision of the prepared steel fiber ceramic composite material and good practicability.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent changes made by using the contents of the present specification and the drawings, or applied directly or indirectly to the related technical fields, are included in the scope of the present invention.

Claims (10)

1. The embedded direct-writing 3D printing preparation method of the steel fiber ceramic composite material is characterized by comprising the following steps of:
s1, preparing ceramic matrix suspension and steel fiber ink;
s2, performing embedded direct-writing 3D printing;
and S3, drying, degreasing and sintering the printed part.
2. The embedded direct-writing 3D printing preparation method of the steel fiber ceramic composite material according to claim 1, wherein S1 specifically comprises the following steps of S11:
dissolving temperature-sensitive hydrogel powder and distilled water in the distilled water according to the mass percent of 25wt% and 30wt% respectively, and storing the solution in an environment at 0-4 ℃ for 24-36 hours to obtain two parts of Pluronic gel with the mass percent of 25wt% and 30wt% respectively.
3. The embedded direct-writing 3D printing preparation method of the steel fiber ceramic composite material according to claim 2, wherein the step S1 specifically comprises the steps of S12:
mixing alumina powder and Pluronic gel with the mass percent of 25wt% according to the weight ratio of 7:3, adding a dispersant with the mass of 1-3% of the mass of the alumina powder to obtain a mixture, and placing the mixture in an ice bath for cooling for 20-30 minutes.
4. The embedded direct-writing 3D printing preparation method of the steel fiber ceramic composite material according to claim 3, wherein the step S1 specifically comprises the steps of S13:
and stirring the cooled mixture for 5-10 minutes at a speed of 2000-2500 rpm, then placing the mixture in an ice bath for cooling for 20-30 minutes, and repeatedly stirring and cooling for 3-5 times to obtain the ceramic matrix suspension.
5. The embedded direct-writing 3D printing preparation method of the steel fiber ceramic composite material according to claim 4, wherein the step S1 specifically comprises the steps of S14:
mixing steel powder and 30wt% of Pluronic gel according to the volume ratio of 1:3, adding 0.5-1.5 wt% of dispersant by weight of the steel powder to obtain a mixture, and placing the mixture in an ice bath for cooling for 20-30 minutes.
6. The embedded direct-writing 3D printing preparation method of the steel fiber ceramic composite material according to claim 5, wherein the step S1 specifically comprises the steps of S15:
and stirring the cooled mixture for 5-10 minutes at a speed of 2000-2500 rpm, then placing the mixture in an ice bath for cooling for 20-30 minutes, and repeating stirring and cooling for 3-5 times to obtain the steel fiber ink.
7. The embedded direct-writing 3D printing preparation method of the steel fiber ceramic composite material according to claim 1, wherein the step S2 specifically comprises the steps of S21:
and respectively placing the ceramic matrix suspension and the steel fiber ink in a vacuum environment for drying for 60-70 minutes.
8. The embedded direct-writing 3D printing preparation method of the steel fiber ceramic composite material according to claim 7, wherein the step S2 specifically comprises the steps of S22:
and cooling the dried ceramic matrix suspension to 0-10 ℃, and pouring the ceramic matrix suspension into a silica gel mold coated with silicone oil.
9. The embedded direct-writing 3D printing preparation method of the steel fiber ceramic composite material according to claim 8, wherein the step S2 specifically comprises the steps of S23:
and (3) placing the silica gel mold in a water bath with the temperature of 15-20 ℃, injecting the steel fiber ink into a needle cylinder for direct-writing 3D printing, and extruding ink filaments with the diameter of 10-700 um by using a nozzle with the inner diameter of 10-600 um.
10. The embedded direct-writing 3D printing preparation method of the steel fiber ceramic composite material according to claim 9, wherein the S3 specifically comprises the steps of:
s31, taking down the silica gel mold containing the ceramic matrix suspension and the printed ink, and drying in an environment with the temperature of 32 ℃ for 1-2 weeks;
s32, taking the dried ceramic matrix suspension out of the silica gel mold, placing the silica gel mold in a sintering furnace, heating the silica gel mold from room temperature to 350 ℃ at the heating rate of 1 ℃/min, preserving heat for 1-2 hours, then continuously heating the silica gel mold to 500 ℃ at the heating rate of 2 ℃/min, preserving heat for 2-3 hours, and then opening the box to cool the silica gel mold to the normal temperature;
and S33, heating the temperature from room temperature to 1550 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 2-3 hours, and finally opening the box and cooling to the normal temperature.
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