CN111056853A - A method for preparing silicon carbide ceramic composite material by using light-cured short carbon fiber as carbon fiber preform - Google Patents
A method for preparing silicon carbide ceramic composite material by using light-cured short carbon fiber as carbon fiber preform Download PDFInfo
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Abstract
本发明涉及一种以光固化短碳纤维为碳纤维预制体制备碳化硅陶瓷复合材料的方法，所述制备碳化硅陶瓷复合材料的方法包括：（1）将短碳纤维和光敏树脂混合，得到光敏浆料；（2）根据预先设计可具复杂结构的碳纤维预制体的三维模型，采用数字光处理光固化3D打印技术，将光敏浆料逐层打印形成三维实体，再经过紫外光固化、清洗和干燥，得到所述碳纤维预制体；（3）将所得碳纤维预制体经过脱粘处理后，得到三维纯碳纤维支架；（4）将所得三维纯碳纤维支架经液相渗硅反应烧结，得到所述碳化硅陶瓷复合材料。
The invention relates to a method for preparing a silicon carbide ceramic composite material by using a photocurable short carbon fiber as a carbon fiber preform. The method for preparing a silicon carbide ceramic composite material includes: (1) mixing the short carbon fiber and a photosensitive resin to obtain a photosensitive slurry ; (2) According to the pre-designed three-dimensional model of carbon fiber preforms with complex structures, using digital light processing and photo-curing 3D printing technology, the photosensitive paste is printed layer by layer to form a three-dimensional entity, and then cured, cleaned and dried by ultraviolet light. obtaining the carbon fiber preform; (3) debonding the obtained carbon fiber preform to obtain a three-dimensional pure carbon fiber support; (4) sintering the obtained three-dimensional pure carbon fiber support through liquid-phase silicon infiltration to obtain the silicon carbide ceramic composite material.
Description
Technical Field
The invention relates to a method for preparing a silicon carbide ceramic composite material, in particular to a method for preparing a silicon carbide ceramic composite material by taking photocuring short carbon fibers as a carbon fiber preform, and belongs to the field of silicon carbide ceramic composite materials.
Background
The silicon carbide ceramic composite material has excellent performances of high specific stiffness, small volume density, high thermal conductivity, high temperature resistance, corrosion resistance, stable chemical performance, thermal shock resistance and the like, and shows important application value and potential in the fields of aerospace, petrochemical industry, automobile parts, microelectronics and the like. At present, the processing and forming mode of the silicon carbide ceramic composite material part mostly adopts the traditional forming technology, such as: dry pressing, slip casting, isostatic pressing, and the like. In the process of preparing the ceramic biscuit, the technologies need to use a mould, so that the forming period of the silicon carbide ceramic product is prolonged, and the manufacturing difficulty of the silicon carbide-based ceramic part with the special-shaped and composite structure is increased. For example, the method of slip casting with carbon fiber and resin mixture to prepare a three-dimensional structure preform requires a complex forming mold, slip casting/pressure curing, and then carbonization, which is complicated in process and long in time consumption, and has certain limitation especially on the preparation of a preform with a complex structure.
With the continuous expansion of the application range of the silicon carbide ceramic composite material part, people have more and more extensive requirements on the silicon carbide ceramic composite material product with the complex structure, and the 3D printing technology is an effective mode for preparing the silicon carbide ceramic part with high precision and the complex structure. Meanwhile, silicon melt can be infiltrated into the ceramic biscuit at high temperature through reaction sintering, and the density and the performance of the ceramic part are improved.
Disclosure of Invention
Aiming at the problems of difficult manufacture and complex processing of the existing silicon carbide ceramic composite material part with the special-shaped complex structure, the invention provides a method for preparing a silicon carbide ceramic composite material by taking photocuring short carbon fiber as a carbon fiber preform, which comprises the following steps:
(1) mixing short carbon fibers and photosensitive resin to obtain photosensitive slurry;
(2) printing photosensitive slurry layer by layer to form a three-dimensional entity by adopting a digital light processing photocuring 3D printing technology according to a three-dimensional model of a carbon fiber preform which is designed in advance and can have a complex structure, and then performing ultraviolet curing, cleaning and drying to obtain the carbon fiber preform;
(3) carrying out debonding treatment on the obtained carbon fiber preform to obtain a three-dimensional pure carbon fiber support;
(4) and sintering the obtained three-dimensional pure carbon fiber support through a liquid phase siliconizing reaction to obtain the silicon carbide ceramic composite material.
In the present invention, the preform prepared by degreasing and 3D printing of short carbon fibers has better structural designability (arbitrary three-dimensional structure), high manufacturing accuracy (25 μm in the vertical direction, horizontal molding deviation < 5%), and high manufacturing efficiency. In fact, 3D printing forming and curing are realized together, a prefabricated body with any three-dimensional structure can be obtained through direct debonding and carbonization, the limitation of forming of a mold is broken through, process flow steps are reduced, and single step is short in time, so that the preparation period of the whole silicon carbide ceramic composite material is greatly shortened. In addition, the carbon fiber/silicon carbide ceramic composite part prepared by the subsequent liquid phase siliconizing sintering has improved compactness, good mechanical property and bending strength close to 300MPa, and the composite material prepared by the method has good application prospect.
Preferably, the mixing mode of the photosensitive paste is ball milling or ultrasonic mixing, and bubbles in the mixed photosensitive paste are removed through vacuum decompression.
Preferably, the diameter of the short carbon fiber is 2-30 μm, and the length is 10-1000 μm; preferably, the length of the short carbon fiber is 10 to 200 μm.
Preferably, the photosensitive resin is selected from resins cured at ultraviolet wavelengths of 395nm or 405nm, and is preferably at least one of an epoxy photosensitive resin, an acrylic photosensitive resin, a polyester photosensitive resin, a polyurethane photosensitive resin, and a thiol-ene photosensitive resin.
Preferably, the volume content of the short carbon fibers in the photosensitive paste is 5-65 vol%.
Preferably, the parameters of the digital light processing photocuring 3D printing technology include: the exposure power is 6-120 mW/cm2The exposure time of the single layer is 1-100 s, and the set layer thickness of the single layer is 10-100 μm.
Preferably, the temperature of the debonding treatment is 500-900 ℃; preferably, the temperature rise rate of the debonding treatment is 1-10 ℃/min, and more preferably < 5 ℃/min.
Preferably, silicon powder which is 1-3 times of the mass of the three-dimensional pure carbon fiber support is weighed and placed around the three-dimensional carbon fiber support to be subjected to liquid phase siliconizing reaction sintering; the parameters of the liquid phase siliconizing reaction sintering comprise: the atmosphere is vacuum atmosphere, the temperature is 1500-1700 ℃, and the time is 0.5-2 hours.
On the other hand, the invention also provides the silicon carbide ceramic composite material prepared by the method, and the components of the silicon carbide ceramic composite material are three phases of silicon carbide, silicon and carbon fiber or two phases of silicon carbide and silicon. Preferably, the bending strength of the silicon carbide ceramic composite material is 30-300 MPa, preferably 180-300 MPa, and more preferably 200-300 MPa.
Has the advantages that:
compared with the traditional forming method for preparing the silicon carbide ceramic composite material, the method for preparing the silicon carbide composite material by using the photocuring carbon fibers as the prefabricated part has the advantages of shorter processing period, simpler post-treatment process and adjustable internal structure and components;
according to the invention, through the early 3D structure design, the light-cured short carbon fiber forming and the subsequent liquid phase siliconizing reaction sintering control, the silicon carbide ceramic composite material with high porosity (see figure 10) can be easily realized, and the substantial silicon carbide ceramic composite material with complicated internal support (see figure 11) can be realized, so that the wider application requirements can be met.
Drawings
FIG. 1 is a structural model of a photo-cured carbon fiber preform obtained in example 1;
FIG. 2 is a representation of a photo-cured carbon fiber preform obtained in example 1;
FIG. 3 is a top view of a photo-cured carbon fiber preform object obtained in example 1;
FIG. 4 is a microstructure of a photo-cured carbon fiber preform obtained in example 1;
FIG. 5 shows the micro-morphology of the photo-cured carbon fiber preform obtained in example 1 after reaction sintering;
FIG. 6 is an XRD pattern of a sintered sample of the photo-cured carbon fiber preform obtained in example 1;
FIG. 7 is a structural model of a photo-cured carbon fiber preform for mechanical property testing obtained in example 1;
FIG. 8 is an object of the photo-cured carbon fiber preform for mechanical property testing obtained in example 1;
FIG. 9 is a high-precision schematic microstructure of a light-cured carbon fiber preform;
FIG. 10 is a high porosity silicon carbide ceramic composite obtained in accordance with the present invention;
FIG. 11 shows the intrinsic silicon carbide ceramic composite material with complex internal support obtained by the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
In the method, the photocuring short carbon fiber is used as a carbon fiber preform for the first time, the silicon carbide ceramic composite material is prepared by combining reaction and sintering, and the structure and the components of the obtained silicon carbide ceramic composite material can be regulated and controlled by the method.
According to the invention, three-dimensional short carbon fibers printed by photocuring 3D are used as a carbon source and a forming framework, a reaction sintering mode is combined, a silicon carbide ceramic composite material part with a complex structure can be prepared without a mould, and the method has the characteristics of simple process, high precision (25-micron layer thickness manufacturing, horizontal forming deviation less than 5%) of a prefabricated body and high-efficiency forming, so that the integral manufacturing period of the silicon carbide ceramic composite material part is shortened. The method for preparing the silicon carbide ceramic composite material by using the photocuring short carbon fiber as the preform is exemplarily described below.
And mixing the short carbon fibers with photosensitive resin to obtain photosensitive slurry. The short carbon fiber and photosensitive resin are used as raw materials to be mixed to prepare photosensitive slurry. Wherein, the diameter of the short carbon fiber is 2-30 μm, the length can be 10-1000 μm, and the preferable length can be 10-200 μm. The ultraviolet light wavelength suitable for the photosensitive resin can be 395nm or 405 nm. The photosensitive resin is at least one selected from the group consisting of an epoxy photosensitive resin, an acrylic photosensitive resin, a polyester photosensitive resin, a polyurethane photosensitive resin, and a thiol-ene photosensitive resin. The content of the short carbon fiber can account for 5-65 vol% of the volume content of the photosensitive paste. In order to disperse uniformly, improve printing precision and increase printability of the photosensitive paste, the photosensitive paste can be mixed by ball milling or ultrasonic mixing, and silicon carbide balls are used as grinding media. The mixed photosensitive paste may be subjected to a vacuum decompression to remove bubbles.
And carrying out photocuring 3D printing, ultraviolet light post-curing (ultraviolet light curing), ultrasonic cleaning and drying on the photosensitive slurry to obtain the photocuring carbon fiber preform. Specifically, the photosensitive paste is transferred into a magazine of a digital light processing photocuring 3D printing device, and according to a designed three-dimensional model (for example, an octagonal truss stacking structure model constructed in the figure 1, the parameters of unit cells of the octagonal truss are L multiplied by W multiplied by H: 2mm multiplied by 2mm, and the diameter of the truss is 0.35mm), the photosensitive paste is solidified layer by layer, and finally, a short carbon fiber support (namely, a three-dimensional entity) with a complex structure is printed. Wherein, in the process of digital light processing photocuring 3D printing, the exposure power can be 6-120 mW/cm2The exposure time of the single layer can be 1-100 s, and the set layer thickness of the single layer can be 10-100 μm. And taking the obtained short carbon fiber support down from a printing equipment forming table, and carrying out post-treatment processes such as ultraviolet curing, ultrasonic cleaning and drying to obtain a photo-cured carbon fiber preform. For example, the post-treatment process may be sequentially: curing for 5min in an ultraviolet curing machine, ultrasonically cleaning for 5min, and drying for 1h in an oven at 60 ℃ to obtain the photocuring carbon fiber preform.
And (4) carrying out debonding treatment on the carbon fiber preform to obtain the three-dimensional pure carbon fiber support. And placing the carbon fiber preform in a graphite crucible, and heating to remove the cured photosensitive resin in the short carbon fiber preform. Wherein, the de-bonding temperature can be 500-900 ℃, the heating rate can be 1-10 ℃/min, and the preferable temperature is less than 5 ℃/min. The heat treatment atmosphere may be a vacuum atmosphere or an inert atmosphere, such as argon.
And (3) sintering the three-dimensional pure carbon fiber bracket through a liquid phase siliconizing reaction (or called liquid phase siliconizing reaction or vacuum liquid phase siliconizing) to obtain the silicon carbide ceramic composite material. Placing the three-dimensional pure carbon fiber support in a graphite crucible coated with boron nitride, weighing silica powder with the mass being 1-3 times that of the three-dimensional pure carbon fiber support, and placing the silica powder around the three-dimensional carbon fiber support. The sintering mode can be liquid phase siliconizing reaction sintering (reaction sintering for short). The atmosphere for the liquid phase siliconizing reaction sintering may be a vacuum atmosphere. The highest set temperature of the liquid phase siliconizing reaction sintering can be 1500-1700 ℃. The reaction sintering heat preservation time can be 0.5-2 h, and the silicon carbide ceramic composite material is prepared.
The obtained silicon carbide ceramic composite material is further processed to test various performances of the silicon carbide ceramic composite material.
In the invention, an energy spectrometer is adopted to measure that the components of the silicon carbide ceramic composite material prepared by taking the photocuring short carbon fiber as the preform comprise three phases of silicon carbide, silicon and carbon fiber or two phases of silicon carbide and silicon under different process conditions. According to the invention, the bending strength of the silicon carbide ceramic composite material prepared by using the photocuring short carbon fiber as the preform is 30-300 MPa by adopting a three-point bending method.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
20.86 vol% of short carbon fiber and 79.14 vol% of photosensitive resin are mixed, silicon carbide balls are used as grinding media, ball milling is carried out for 15min at the rotating speed of 1500rad/s, and vacuum decompression and degassing are carried out for 2min to prepare photosensitive slurry. Then, according to the designed composite structure model (shown in FIG. 1), the exposure power was 88.00mW/cm2The single-layer exposure time is 60s, the single-layer set layer thickness is 25 microns, the single-layer set layer thickness is cured for 2min after ultraviolet light, ultrasonic cleaning is carried out for 5min, drying is carried out in an oven at 60 ℃ for 1h, a carbon fiber preform (shown in figure 2) is obtained, the microstructure of the carbon fiber preform is shown in figures 3 and 4 and is a complex periodic grid structure, the carbon fiber preform is subjected to debonding treatment at 700 ℃ to obtain a three-dimensional pure carbon fiber support, the three-dimensional pure carbon fiber support is placed in a graphite crucible coated with boron nitride, silicon powder with the mass twice as large as that of the support is weighed and placed around the support, vacuum liquid phase siliconizing is carried out at 1650 ℃, densification is realized after heat preservation for 1h, and cooling is carried out in an argon environment to obtain a silicon carbide ceramic composite material, the microstructure and the components of the obtained silicon carbide ceramic composite material are shown in figures 5 and 6, the components of the original carbon fiber support are uniformly distributed, the silicon carbide ceramic composite material is β -silicon carbide, the silicon and is completely filled with the original holes, the mechanical properties of the silicon carbide ceramic composite material are further tested, and the mechanical properties of the silicon carbide ceramic composite material are obtained by adopting.
Example 2
20.86 vol% of short carbon fiber and 79.14 vol% of photosensitive resin are mixed, silicon carbide balls are used as grinding media, ball milling is carried out for 15min at the rotating speed of 1500rad/s, and vacuum decompression and degassing are carried out for 2min to prepare photosensitive slurry. Then, according to the designed composite structure model (FIG. 1), the exposure power was 88.00mW/cm2And carrying out ultraviolet light post-curing for 2min, carrying out ultrasonic cleaning for 5min, and drying in an oven at 60 ℃ for 1h to obtain the carbon fiber preform, wherein the single-layer exposure time is 60s, and the set layer thickness of the single layer is 50 microns. Mixing carbon fiberThe preparation method comprises the steps of carrying out debonding treatment on a prefabricated body at 700 ℃ to obtain a three-dimensional pure carbon fiber support, placing the three-dimensional pure carbon fiber support in a graphite crucible coated with boron nitride, weighing silicon powder with twice the mass of the support around the support, carrying out vacuum liquid phase siliconizing at 1600 ℃, carrying out heat preservation for 0.5h to realize densification, and carrying out cooling in an argon environment to obtain a silicon carbide ceramic composite material, wherein the components of the position of the original carbon fiber support are uniformly distributed and are β -silicon carbide, silicon and carbon fiber, and the original holes are completely filled with silicon.
Example 3
15.68 vol% of short carbon fiber and 84.32 vol% of photosensitive resin are mixed, silicon carbide balls are used as grinding media, ball milling is carried out for 15min at the rotating speed of 1500rad/s, and vacuum decompression and degassing are carried out for 2min to prepare photosensitive slurry. Then, according to the designed composite structure model (FIG. 1), the exposure power was 88.00mW/cm2The preparation method comprises the steps of setting the exposure time of a single layer to be 60s, setting the layer thickness of the single layer to be 25 microns, curing for 2min after ultraviolet light, carrying out ultrasonic cleaning for 5min, drying for 1h in an oven at 60 ℃ to obtain a carbon fiber preform, carrying out debonding treatment on the carbon fiber preform at 700 ℃ to obtain a three-dimensional pure carbon fiber support, placing the three-dimensional pure carbon fiber support in a graphite crucible coated with boron nitride, weighing silicon powder with twice the mass of the support around the support, carrying out vacuum liquid-phase siliconizing at 1650 ℃, carrying out heat preservation for 1h to realize densification, cooling in an argon environment to obtain a silicon carbide ceramic composite material, and obtaining the silicon carbide ceramic composite material after sintering, wherein the position components of the original carbon fiber support are uniformly distributed, namely β -silicon carbide, silicon and carbon fiber three phases, and the original holes are completely filled with silicon.
Example 4
15.68 vol% of short carbon fiber and 84.32 vol% of photosensitive resin are mixed, silicon carbide balls are used as grinding media, and the balls are rotated at 1500rad/sGrinding for 15min, and vacuum degassing for 2min to obtain photosensitive slurry. Then, according to the designed composite structure model (FIG. 1), the exposure power was 88.00mW/cm2The preparation method comprises the steps of setting the exposure time of a single layer to be 60s, setting the layer thickness of the single layer to be 50 microns, curing for 2min after ultraviolet light, carrying out ultrasonic cleaning for 5min, drying for 1h in an oven at 60 ℃ to obtain a carbon fiber preform, carrying out debonding treatment on the carbon fiber preform at 700 ℃ to obtain a three-dimensional pure carbon fiber support, placing the three-dimensional pure carbon fiber support in a graphite crucible coated with boron nitride, weighing silicon powder with twice the mass of the support around the support, carrying out vacuum liquid phase siliconizing at 1600 ℃, carrying out heat preservation for 0.5h to realize densification, cooling in an argon environment to obtain a silicon carbide ceramic composite material, and carrying out sintering on the silicon carbide ceramic composite material, wherein the position components of the original carbon fiber support are uniformly distributed and are β -three phases of silicon carbide, silicon and carbon fiber, and the original hole is completely filled with silicon.
Example 5
See example 1 for a process for preparing a silicon carbide ceramic composite material of example 5, except that: the quality of the added silicon powder is the same as that of the three-dimensional pure carbon fiber bracket.
Example 6
See example 1 for a process for preparing a silicon carbide ceramic composite material of example 6, except that: the mass of the added silicon powder is 3 times of that of the three-dimensional pure carbon fiber bracket.
Table 1 shows the preparation process and performance parameters of the silicon carbide ceramic composite material prepared according to the present invention:
Claims (9)
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| CN114890425A (en) * | 2022-04-02 | 2022-08-12 | 西安交通大学 | Elastic silicon carbide nanowire aerogel with multilevel structure and 3D printing preparation method and application thereof |
| CN115286408A (en) * | 2022-08-17 | 2022-11-04 | 中国科学院上海硅酸盐研究所 | A method for preparing silicon carbide composite parts by laser 3D printing based on particle gradation composite technology |
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| CN114890425B (en) * | 2022-04-02 | 2023-12-19 | 西安交通大学 | A multi-level structure elastic silicon carbide nanowire aerogel and its 3D printing preparation method and application |
| CN115286408A (en) * | 2022-08-17 | 2022-11-04 | 中国科学院上海硅酸盐研究所 | A method for preparing silicon carbide composite parts by laser 3D printing based on particle gradation composite technology |
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