CN115745570A - Porous ceramic with gradient pore structure framework and 3D printing forming method thereof - Google Patents
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Abstract
The invention discloses porous ceramic with a gradient pore structure framework and a 3D printing forming method thereof, and relates to the technical field of porous ceramic materials. The method comprises the following steps: respectively mixing the hollow microspheres with different particle size distributions with ceramic powder, water, a dispersing agent and protein powder to obtain ceramic slurry with the hollow microspheres with different particle sizes, defoaming, performing 3D printing on the ceramic slurry with the hollow microspheres with different particle sizes according to a certain hollow microsphere particle size sequence, drying, discharging glue, sintering, and cooling along with a furnace to obtain the ceramic slurry. According to the invention, the porous ceramic with the gradient pore structure framework is prepared by controlling the printing sequence of the hollow microspheres with different particle sizes, the rapid regulation and control of the internal pore structure of the three-dimensional framework of the porous ceramic are realized, the method is simple and effective, the ceramic product with a complex shape can be prepared, the method has important significance for the microstructure and function regulation and control of 3D printing porous ceramic, and the application of the 3D printing technology in various fields can be effectively expanded.
Description
Technical Field
The invention relates to the technical field of porous ceramic materials, in particular to porous ceramic with a gradient pore structure framework and a 3D printing forming method thereof.
Background
The porous ceramic is used as a light material with high porosity, has the characteristics of high temperature resistance, corrosion resistance, aging resistance, high chemical stability and the like, and is widely applied to the fields of aviation and aerospace thermal protection, biological bones, filters, heat exchangers, fuel combustion, sound absorption and noise reduction, energy storage devices and the like. The 3D printing manufacturing technology is a one-door system and comprehensive technology, covers multidisciplinary knowledge such as computer software, material science, mechanical manufacturing, automatic control, network information and the like, and is a new technology in the field of manufacturing industry. The preparation of the porous ceramic is realized by using the 3D printing technology without the restriction of a mould and a shape, subsequent cutting processing is not required or the subsequent processing amount is less, parts and products with complex characteristics, which are difficult to prepare by using a traditional processing mode, can be prepared, raw materials can be effectively saved, and the material cost of the products is reduced. At present, the fields such as aerospace, biomedical, teaching and scientific research, automobile industry and the like all have the application of 3D printing technology, play more and more important role, and the deep research on the 3D printing technology is increasingly concerned by researchers.
The optimization of various properties of the porous ceramic material by fine control of the microstructure of the material is an important research direction. At present, 3D printing material mainly adjusts printing diameter, sample shape, skeleton layer height etc. through setting up model design and printer parameter, lacks the regulation and control to skeleton self microstructure. The functional gradient material is a composite material with the composition structure and the performance changing in a gradient (including a hierarchical gradient and a continuous gradient) on the thickness or the length of the material, can combine the advantages of different types of materials according to the design requirement to prepare the material with excellent performance, and has obvious advantages different from the conventional material.
Disclosure of Invention
The invention aims to provide porous ceramic with a gradient pore structure framework and a 3D printing forming method thereof, which are used for solving the problems in the prior art and realizing effective regulation and control of a porous ceramic pore structure.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a 3D printing forming method of porous ceramic with a gradient pore structure framework, which comprises the following steps:
(1) Respectively mixing the hollow microspheres with different particle size distributions with ceramic powder, deionized water, an ammonium citrate dispersant and albumen powder to obtain ceramic slurry with the hollow microspheres with different particle sizes;
(2) Defoaming the ceramic slurry with the hollow microspheres with different particle sizes;
(3) And 3D printing the ceramic slurry with the hollow microspheres with different particle sizes according to the particle size sequence of the hollow microspheres, drying the obtained blank (at 40-60 ℃, the drying time is more than or equal to 6 hours), discharging the glue, sintering, and cooling along with the furnace to obtain the porous ceramic with the gradient pore structure framework.
Further, the hollow microspheres are fly ash hollow microspheres and Al 2 O 3 Hollow microspheres, siO 2 Hollow microspheres and ZrO 2 One or more of the hollow microspheres.
The hollow microspheres are screened by a standard sieve to obtain microspheres with specific particle size ranges, such as 80-100 meshes (150-200 mu m), 100-120 meshes (125-150 mu m), 120-160 meshes (97-125 mu m), 160-200 meshes (97-75 mu m), 200-300 meshes (54-75 mu m) and 300-500 meshes (54-25 mu m).
Further, the ceramic powder is aluminum silicate powder and Al 2 O 3 、SiO 2 And ZrO 2 One or more of (2), the particle size of the powder is 1-10 mu m.
Furthermore, the mass ratio of the hollow microspheres to the ceramic powder, water, dispersant and protein powder is 27-33.
Further, the degree of vacuum in the defoaming treatment is 0.6kPa or less, and the defoaming time is 5 to 15min.
Further, the 3D printing mode in the step (3) is direct-write printing, and the printing speed is 5-30 mm/s.
And (3) pouring the defoamed various types of ceramic slurry into different printing raw material tanks in the printing process, sequentially selecting the corresponding printing raw material tanks according to the order of the particle sizes of the hollow spheres from small to large for 3D printing, placing the ceramic blank with the gradient pore structure skeleton obtained after printing in an oven for drying, and removing glue and sintering at high temperature to obtain the porous ceramic with the gradient pore structure skeleton.
Specifically, the method comprises the following steps: the method comprises the steps that a 3D printer is utilized to firstly carry out direct-writing printing on ceramic slurry with the smallest hollow sphere particle size according to a designed blank body framework structure, after the previous type of ceramic slurry is printed, a raw material tank of the next type of hollow sphere ceramic slurry is replaced according to the sequence of the particle sizes from small to large, and printing is continuously carried out on the basis of the blank body until the printing is finished.
Further, the temperature of the rubber discharge is 600 ℃, and the time is 1-2 h; the sintering temperature is 1250-1550 ℃ and the sintering time is 2-6 h.
Further, the heating rate of the binder removal and sintering is 2-5 ℃/min.
The invention further provides the porous ceramic with the gradient pore structure skeleton, which is prepared by the 3D printing and forming method.
Ceramic hollow microsphere (SiO) 2 、ZrO 2 、Al 2 O 3 、TiO 2 Etc.) has the advantages of light weight and high strength in addition to the inherent characteristics of high temperature resistance, corrosion resistance, good thermal stability and the like of ceramic materials. According to the invention, the hollow microspheres are used as raw materials and combined with the 3D printing technology to regulate and control the three-dimensional skeleton micro-pore structure of the ceramic material, the porous ceramic with the gradient pore structure skeleton is prepared by controlling the granularity of the hollow microspheres, and the porous ceramic has important significance for regulating and controlling the microstructure and functions of the 3D printing porous ceramic, and can effectively expand the application of the 3D printing technology in various fields.
The invention discloses the following technical effects:
according to the invention, the hollow microspheres and a 3D printing technology are combined, the hollow microspheres with different particle size ranges are obtained by screening through a standard screen and are used as raw materials, and the porous ceramic with the gradient pore structure framework is prepared by controlling the printing sequence of the hollow microspheres with different particle sizes, so that the rapid regulation and control of the internal pore structure of the three-dimensional porous ceramic framework are realized, the method is simple and effective, and the ceramic product with a complex shape can be prepared. The method has important significance for the microstructure and function regulation of the 3D printing porous ceramic, and can effectively expand the application of the 3D printing technology in various fields. In addition, the hollow ceramic microspheres in the three-dimensional skeleton of the porous ceramic can further reduce the overall density of the porous ceramic, are beneficial to ultra-lightening of the porous ceramic, and have important research and application values.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is an optical diagram of a printing process of a porous ceramic having a skeletal structure with a gradient pore structure according to example 1 of the present invention;
FIG. 2 is an optical diagram of a porous ceramic having a gradient pore structure skeleton printed in example 1 of the present invention;
FIG. 3 is a microscopic morphology of a cross section of a three-dimensional skeleton of a 300-1000 mesh (15-54 μm) layer in the porous ceramic prepared by 3D printing in example 1 of the present invention;
FIG. 4 is a micro-topography of a cross section of a three-dimensional skeleton of a 160-300 mesh (54-97 μm) layer in the porous ceramic prepared by 3D printing in example 1 of the present invention;
FIG. 5 is a microscopic morphology of a cross section of a three-dimensional skeleton of a 100-160 mesh (97-150 μm) layer in the porous ceramic prepared by 3D printing in example 1 of the present invention;
FIG. 6 is a microscopic morphology of a cross section of a three-dimensional skeleton of 80-100 mesh (150-200 μm) layer in the porous ceramic prepared by 3D printing in example 1 of the present invention.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
Example 1
Preparing the porous ceramic with the framework with the gradient pore structure:
(1) The method comprises the following steps of screening by using a standard sieve to obtain the fly ash hollow microspheres with the particle sizes of 80-100 meshes (150-200 mu m), 100-160 meshes (97-150 mu m), 160-300 meshes (54-97 mu m) and 300-1000 meshes (15-54 mu m), and mixing the fly ash hollow microspheres, the ceramic powder, the deionized water, the ammonium citrate dispersant and the protein powder in a mass ratio of 28.
(2) Pouring various types of ceramic slurry into a centrifugal tank with an opening at the top, and then placing the centrifugal tank into a vacuum defoaming machine (the vacuum degree is set to be 0.5kPa, and the defoaming time is set to be 10 min) to carry out defoaming treatment on the ceramic slurry.
(3) After defoaming, firstly, selecting 300-1000-mesh hollow microsphere ceramic slurry and printing by using a direct-writing 3D printer, wherein the printing speed is 10mm/s, and the number of printing layers is 3; then, the blank is replaced by the hollow microsphere ceramic slurry with the mesh size of 160-300, and the blank is continuously printed at the printing speed of 10mm/s and 3 layers; and then, repeating the printing process by using the hollow microsphere ceramic slurry of 100-160 meshes and 80-100 meshes (the printing speed is 10mm/s, and the number of printing layers is 3), and obtaining a final ceramic blank.
(4) And (3) performing degumming on the ceramic blank dried for 10 hours at the temperature of 40 ℃ for 1 hour at the temperature of 600 ℃, and then sintering the ceramic blank for 4 hours at the temperature of 1450 ℃, wherein the heating rates of the degumming and the sintering processes are both 2 ℃/min. And after sintering, cooling the sintered ceramic along with the furnace to obtain the porous ceramic with the gradient pore structure framework.
Fig. 1 is an optical diagram of a printing process of the porous ceramic of this embodiment, fig. 2 is an optical diagram of the porous ceramic with a gradient pore structure skeleton printed in this embodiment, and fig. 3 to 6 are respectively a micro-topography of a three-dimensional skeleton section of a hollow microsphere layer with different particle size distributions in the porous ceramic of this embodiment.
The pore structure of the three-dimensional framework formed by 3D printing is innovated, gradient change of the pore structure in the three-dimensional framework can be realized, and correspondingly, the change of the mechanical strength from the bottom layer to the top layer of the sample is 4.7MPa → 3.5MPa, and the change of the thermal conductivity is 0.38 W.m -1 ·K -1 →0.32W·m -1 ·K -1 The material has the density, mechanical strength and thermal conductivity of gradient distribution, and can be used as a light high-strength heat insulation material, a ceramic separation membrane and the like.
Example 2
Preparing the porous ceramic with the framework with the gradient pore structure:
(1) The method comprises the following steps of screening by using a standard sieve to obtain the fly ash hollow microspheres with the particle sizes of 100-120 meshes (125-150 mu m), 120-160 meshes (97-125 mu m), 160-200 meshes (75-97 mu m) and 200-300 meshes (54-75 mu m), and mixing the fly ash hollow microspheres, the ceramic powder, the deionized water, the ammonium citrate dispersant and the protein powder according to a mass ratio of 30.
(2) Pouring various types of ceramic slurry into a centrifugal tank with an opening at the top, and then placing the centrifugal tank into a vacuum defoaming machine (the vacuum degree is set to be 0.5kPa, and the defoaming time is set to be 5 min) to carry out defoaming treatment on the ceramic slurry.
(3) After defoaming, firstly, selecting 200-300-mesh hollow microsphere ceramic slurry and printing by using a direct-writing 3D printer, wherein the printing speed is 10mm/s, and the number of printing layers is 5; then, the blank is replaced by the hollow microsphere ceramic slurry with the mesh size of 160-200 meshes, and the blank is continuously printed at the printing speed of 10mm/s and 5 layers; and then, repeating the printing process by using the hollow microsphere ceramic slurry with the meshes of 120-160 and 100-120 (the printing speed is 10mm/s, and the number of printing layers is 5), and obtaining a final ceramic blank.
(4) And (3) carrying out gel discharging on the ceramic blank dried for 9h at the temperature of 45 ℃ for 1h at the temperature of 600 ℃, then sintering the ceramic blank at 1350 ℃ for 4h, wherein the heating rates of the gel discharging and sintering processes are both 4 ℃/min. And after sintering, cooling the sintered ceramic along with the furnace to obtain the porous ceramic with the gradient pore structure framework. The obtained sample has a mechanical strength change from bottom layer to top layer of 4.4MPa → 3.7MPa and a thermal conductivity change of 0.37 W.m -1 ·K -1 →0.33W·m -1 ·K -1 。
Example 3
Preparing porous ceramic with a framework with a gradient pore structure:
(1) The method comprises the following steps of screening by using a standard sieve to obtain the fly ash hollow microspheres with the particle sizes of 120-160 meshes (97-125 microns), 160-200 meshes (75-97 microns), 200-300 meshes (54-75 microns) and 300-500 meshes (25-54 microns), and mixing the fly ash hollow microspheres, the ceramic powder, the deionized water, the ammonium citrate dispersant and the protein powder according to the mass ratio of 27.
(2) Pouring the various types of ceramic slurry into a centrifugal tank with an opening at the top, and then placing the centrifugal tank into a vacuum defoaming machine (the vacuum degree is set to be 0.4kPa, and the defoaming time is set to be 5 min) to carry out defoaming treatment on the ceramic slurry.
(3) After defoaming, firstly, selecting 300-500-mesh hollow microsphere ceramic slurry and printing by using a direct-writing 3D printer, wherein the printing speed is 5mm/s, and the number of printing layers is 5; then, the blank is continuously printed by replacing the hollow microsphere ceramic slurry with 200-300 meshes, the printing speed is 5mm/s, and the number of printing layers is 4; and then repeating the printing process by using the hollow microsphere ceramic slurry with 160-200 meshes and 120-160 meshes (the printing speed is 10mm/s, and the number of the printing layers is 3 and 2 respectively) to obtain a final ceramic blank body.
(4) And (3) carrying out gel discharging on the ceramic blank dried for 8 hours at the temperature of 55 ℃ for 1 hour at the temperature of 600 ℃, then sintering the ceramic blank for 4 hours at the temperature of 1550 ℃, wherein the heating rates of the gel discharging and sintering processes are both 4 ℃/min. And after sintering, cooling the sintered product along with the furnace to obtain the porous ceramic with the gradient pore structure skeleton. The obtained sample has a mechanical strength change from bottom layer to top layer of 4.7MPa → 3.9MPa and a thermal conductivity change of 0.37 W.m -1 ·K -1 →0.34W·m -1 ·K -1 。
Example 4
Preparing porous ceramic with a framework with a gradient pore structure:
(1) The method comprises the following steps of screening by using a standard sieve to obtain the fly ash hollow microspheres with the particle sizes of 80-100 meshes (150-200 mu m), 100-120 meshes (125-150 mu m), 120-160 meshes (97-125 mu m) and 160-200 meshes (75-97 mu m), and mixing the fly ash hollow microspheres, the ceramic powder, the deionized water, the ammonium citrate dispersant and the protein powder according to the mass ratio of (32).
(2) Pouring various types of ceramic slurry into a centrifugal tank with an opening at the top, and then placing the centrifugal tank into a vacuum defoaming machine (the vacuum degree is set to be 0.4kPa, and the defoaming time is set to be 10 min) to carry out defoaming treatment on the ceramic slurry.
(3) After defoaming, firstly, 160-200 meshes of hollow microsphere ceramic slurry is selected and printed by a direct-writing 3D printer, the printing speed is 15mm/s, and the number of printing layers is 2; then, the blank is continuously printed by replacing the hollow microsphere ceramic slurry with 120-160 meshes, the printing speed is 15mm/s, and the number of printing layers is 3; and then, repeating the printing process by using the hollow microsphere ceramic slurry of 100-120 meshes and 80-100 meshes (the printing speed is 15mm/s, and the number of printing layers is 4 and 5 respectively) to obtain the final ceramic blank.
(4) Gelatinizing ceramic blank dried at 50 deg.C for 10 hr at 600 deg.C for 1 hr, and then firing at 1250 deg.CAnd 4h, setting the temperature rise rate in the binder removal and sintering processes to be 2 ℃/min. And after sintering, cooling the sintered ceramic along with the furnace to obtain the porous ceramic with the gradient pore structure framework. The sample has a mechanical strength change from the bottom layer to the top layer of 4.2MPa → 3.5MPa and a thermal conductivity change of 0.35 W.m -1 ·K -1 →0.32W·m -1 ·K - 1。
According to the invention, the ceramic hollow microspheres are combined with a 3D printing technology, the hollow microspheres with different particle size ranges are obtained by screening through a standard screen and are used as raw materials, and the porous ceramic with the gradient pore structure framework is prepared by controlling the printing sequence, so that the rapid regulation and control of the internal pore structure of the three-dimensional framework of the porous ceramic are realized, the method is simple and effective, and the ceramic product with a complex shape can be prepared. The method has important significance for the microstructure and the function regulation of the 3D printing porous ceramic, and can effectively expand the application of the 3D printing technology in various fields. In addition, the hollow ceramic microspheres in the three-dimensional skeleton of the porous ceramic can further reduce the overall density of the porous ceramic, are beneficial to ultra-lightening of the porous ceramic, and have important research and application values.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (9)
1. A3D printing forming method of porous ceramics with a gradient pore structure framework is characterized by comprising the following steps:
(1) Respectively mixing the hollow microspheres with different particle size distributions with ceramic powder, water, a dispersing agent and protein powder to obtain ceramic slurry with the hollow microspheres with different particle sizes;
(2) Respectively defoaming the ceramic slurry with the hollow microspheres with different particle sizes;
(3) And 3D printing the ceramic slurry with the hollow microspheres with different particle sizes according to a certain hollow microsphere particle size sequence, drying, removing the glue, sintering the obtained blank, and cooling along with a furnace to obtain the porous ceramic with the gradient pore structure framework.
2. The 3D printing and forming method according to claim 1, wherein the hollow microspheres are coal ash hollow microspheres and Al 2 O 3 Hollow microsphere, siO 2 Hollow microspheres and ZrO 2 One or more of the hollow microspheres.
3. The 3D printing and forming method according to claim 1, wherein the ceramic powder is aluminum silicate powder and Al 2 O 3 、SiO 2 And ZrO 2 The particle size of the powder is 1-10 mu m.
4. The 3D printing and forming method according to claim 1, wherein the mass ratio of the hollow microspheres to the ceramic powder, water, the dispersing agent and the protein powder is 27-33.
5. The 3D printing and forming method according to claim 1, wherein the vacuum degree in the defoaming treatment is less than or equal to 0.6kPa, and the defoaming time is 5-15 min.
6. The 3D printing forming method according to claim 1, wherein the 3D printing mode in the step (3) is direct-write printing, and the printing speed is 5-30 mm/s.
7. The 3D printing and forming method according to claim 1, wherein the temperature of the rubber discharge is 600 ℃, and the time is 1-2 hours; the sintering temperature is 1250-1550 ℃ and the sintering time is 2-6 h.
8. The 3D printing and forming method according to claim 1, wherein the heating rate of the binder removal and sintering is 2-5 ℃/min.
9. The porous ceramic with the framework of the gradient pore structure, which is prepared by the 3D printing and forming method according to any one of claims 1 to 8.
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