CN115745570B - Porous ceramic with gradient pore structure framework and 3D printing forming method thereof - Google Patents
Porous ceramic with gradient pore structure framework and 3D printing forming method thereof Download PDFInfo
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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: and (3) mixing the hollow microspheres with different particle size distributions with ceramic powder, water, a dispersing agent and protein powder respectively to obtain ceramic slurry with the hollow microspheres with different particle sizes, carrying out 3D printing on the ceramic slurry with the hollow microspheres with different particle sizes according to a certain hollow microsphere particle size sequence after defoaming treatment, drying, discharging glue, sintering and cooling along with a furnace to obtain the ceramic composite material. According to the invention, the porous ceramic with the gradient pore structure skeleton is prepared by controlling the printing sequence of hollow microspheres with different particle diameters, so that the rapid regulation and control of the pore structure inside the three-dimensional skeleton of the porous ceramic is realized, the method is simple and effective, ceramic products with complex shapes can be prepared, the method has important significance for the microstructure and function regulation and control of the 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, ageing resistance, high chemical stability and the like, and is widely applied to the fields of aerospace thermal protection, biological bones, filters, heat exchangers, fuel combustion, sound absorption, noise reduction, energy storage devices and the like. The 3D printing manufacturing technology is taken as a systematic and comprehensive technology, covers multiple disciplinary knowledge such as computer software, material science, mechanical manufacturing, automatic control, network information and the like, and is an emerging technology in the manufacturing industry field. The preparation of the porous ceramic is realized by utilizing the 3D printing technology without being limited by a die and a shape, subsequent cutting processing is not needed or the subsequent processing amount is small, parts and products with complex characteristics which are difficult to prepare in the traditional processing mode can be prepared, raw materials can be effectively saved, and the material cost of the products is reduced. Currently, the 3D printing technology is applied in the fields of aerospace, biomedical science, teaching and scientific research, automobile industry and the like, plays an increasingly important role, and deep research on the 3D printing technology is also increasingly focused by researchers.
The optimization of various properties of the porous ceramic material through fine regulation of the microstructure of the material is an important research direction. Currently, 3D printing materials mainly adjust printing diameter, sample shape, skeleton layer height, etc. through model design and printer parameter settings, lacking in regulation of the skeleton self microstructure. Functionally graded materials are composite materials whose composition structure and properties vary in gradients (including hierarchical gradients, continuous gradients) across the thickness or length of the material, which can combine the advantages of different types of materials according to design requirements to produce materials with superior properties, with significant advantages over conventional materials.
Disclosure of Invention
The invention aims to provide porous ceramic with a gradient pore structure framework and a 3D printing forming method thereof, so as to solve the problems in the prior art and realize effective regulation and control of a pore structure of the porous ceramic.
In order to achieve the above object, the present invention provides the following solutions:
the invention provides a 3D printing forming method of porous ceramics with a gradient pore structure framework, which comprises the following steps:
(1) Mixing hollow microspheres with different particle size distributions with ceramic powder, deionized water, ammonium citrate dispersing agent and protein powder respectively 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 respectively;
(3) 3D printing is carried out on the ceramic slurry with the hollow microspheres with different particle sizes according to the sequence of the particle sizes of the hollow microspheres, and the obtained green body is dried (the drying time is more than or equal to 6h at the temperature of 40-60 ℃), discharged with glue and sintered and then cooled along with a furnace to obtain the porous ceramic with the gradient pore structure skeleton.
Further, the hollow microsphere is a fly ash hollow microsphere and Al 2 O 3 Hollow microsphere, 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(s) 2 The particle size of the powder is 1-10 mu m.
Further, the mass ratio of the hollow microspheres to the ceramic powder, the water, the dispersing agent and the protein powder is 27-33:27-33:34-40:0.3-0.9:2.4-7.2.
Further, the vacuum degree during the defoaming treatment is below 0.6kPa, and the defoaming time is 5-15 min.
Further, in the step (3), the 3D printing mode is direct-writing printing, and the printing speed is 5-30 mm/s.
And (3) pouring the ceramic slurry with the defoaming property into different printing raw material tanks in the printing process, sequentially selecting corresponding printing raw material tanks according to the order of the hollow spherical particle size from small to large for 3D printing, drying the ceramic blank with the gradient pore structure skeleton in an oven, and performing glue discharging and high-temperature sintering to obtain the porous ceramic with the gradient pore structure skeleton.
Specific: and (3) performing direct-writing printing on the ceramic slurry with the smallest hollow sphere particle size according to a designed green body framework structure by utilizing a 3D printer, and continuously printing a raw material tank for replacing the ceramic slurry with the next hollow sphere according to the sequence from small particle size to large particle size after the printing of the previous ceramic slurry is finished until the printing is finished.
Further, the temperature of the glue discharging 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 temperature rising rate of the glue discharging and sintering is 2-5 ℃/min.
The invention further provides porous ceramics with a gradient pore structure skeleton, which are prepared by the 3D printing forming method.
Ceramic hollow microsphere (SiO) 2 、ZrO 2 、Al 2 O 3 、TiO 2 Etc.) not only has the inherent characteristics of high temperature resistance, corrosion resistance, good thermal stability, etc., but also has the advantages of light weight and high strength. According to the invention, the hollow microspheres are used as raw materials and are combined with the 3D printing technology so as to regulate and control the three-dimensional skeleton micro-pore structure of the ceramic material, and the preparation of the porous ceramic with the gradient pore structure skeleton by controlling the granularity of the hollow microspheres has important significance for regulating and controlling the microstructure and the function of the 3D printing porous ceramic, so that the application of the 3D printing technology in various fields can be effectively expanded。
The invention discloses the following technical effects:
according to the invention, the hollow microspheres are combined with a 3D printing technology, the hollow microspheres with different particle size ranges are obtained by screening through a standard sieve, the porous ceramic with the gradient pore structure skeleton is prepared by controlling the printing sequence of the hollow microspheres with different particle sizes, the rapid regulation and control of the pore structure inside the porous ceramic three-dimensional skeleton is realized, and the method is simple and effective, and ceramic products with complex shapes can be prepared. Has important significance for 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, is favorable for the ultra-light weight of the porous ceramic, and has 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 that are 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 other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an optical view of a porous ceramic printing process with a gradient pore structure framework in example 1 of the present invention;
FIG. 2 is an optical view of a porous ceramic with a gradient pore structure skeleton printed in example 1 of the present invention;
FIG. 3 is a microscopic morphology of a 300-1000 mesh (15-54 μm) three-dimensional skeletal section in a porous ceramic prepared by 3D printing in example 1 of the present invention;
FIG. 4 is a microscopic morphology of a 160-300 mesh (54-97 μm) three-dimensional skeleton cross section in a porous ceramic prepared by 3D printing in example 1 of the present invention;
FIG. 5 is a microscopic morphology of a 100-160 mesh (97-150 μm) three-dimensional skeletal section of a porous ceramic prepared by 3D printing in example 1 of the present invention;
FIG. 6 is a microstructure of a three-dimensional skeletal section of 80 to 100 mesh (150 to 200 μm) layers in a porous ceramic prepared by 3D printing in example 1 of the present invention.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions 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. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, 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 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 invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
Example 1
Preparing porous ceramics with a gradient pore structure framework:
(1) The flyash hollow microspheres with the grain diameters 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) are obtained by screening through a standard sieve, and the flyash hollow microspheres, the ceramic powder, the deionized water, the ammonium citrate dispersing agent and the protein powder with the mass ratio of 28:28:37:0.8:3.5 are mixed and then are rotated and stirred uniformly, so that the multi-type ceramic slurry with the hollow microspheres with different grain diameters is obtained.
(2) Pouring each ceramic slurry into a centrifugal tank with an opening at the top, and then placing the ceramic slurry into a vacuum defoaming machine (the set vacuum degree is 0.5kPa, and the defoaming time is 10 min) to perform defoaming treatment on the ceramic slurry.
(3) After defoaming is finished, firstly, hollow microsphere ceramic slurry with 300-1000 meshes is selected and printed by a direct-writing type 3D printer, the printing speed is 10mm/s, and the number of printing layers is 3; then the hollow microsphere ceramic slurry with 160-300 meshes is replaced, printing is continued on the basis of the blank, the printing speed is 10mm/s, and the number of printing layers is 3; and repeating the printing process (the printing speed is 10mm/s and the printing layer number is 3) by using the hollow microsphere ceramic slurry with 100-160 meshes and 80-100 meshes to obtain a final ceramic blank.
(4) And (3) discharging glue from the ceramic blank dried for 10 hours at the temperature of 40 ℃ for 1 hour at the temperature of 600 ℃, and then sintering for 4 hours at the temperature of 1450 ℃, wherein the heating rate of the glue discharging and sintering process is 2 ℃/min. And cooling along with the furnace after sintering to obtain the porous ceramic with the gradient pore structure framework.
Fig. 1 is an optical diagram of a porous ceramic printing process in this embodiment, fig. 2 is an optical diagram of a porous ceramic with a gradient pore structure skeleton printed in this embodiment, and fig. 3 to 6 are microscopic morphologies of three-dimensional skeleton sections of hollow microsphere layers with different particle size distributions in the porous ceramic in this embodiment, respectively.
By innovating the pore structure of the 3D printing molding three-dimensional framework, the gradient change of the pore structure in the three-dimensional framework can be realized, and correspondingly, the mechanical strength change from the bottom layer to the top layer of the sample is 47MPa to 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 gradient distribution density, mechanical strength and thermal conductivity, and can be used as a light high-strength heat insulation material, a ceramic separation membrane and the like.
Example 2
Preparing porous ceramics with a gradient pore structure framework:
(1) The flyash hollow microspheres with the grain diameters 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) are obtained by screening through a standard sieve, and the flyash hollow microspheres, the ceramic powder, the deionized water, the ammonium citrate dispersing agent and the protein powder with the mass ratio of 30:30:38:0.6:3 are mixed and then are rotated and stirred uniformly to obtain the multi-type ceramic slurry with the hollow microspheres with different grain diameters.
(2) Pouring each ceramic slurry into a centrifugal tank with an opening at the top, and then placing the ceramic slurry into a vacuum defoaming machine (the set vacuum degree is 0.5kPa, and the defoaming time is 5 minutes) to perform defoaming treatment on the ceramic slurry.
(3) After defoaming is finished, firstly, hollow microsphere ceramic slurry with 200-300 meshes is selected and printed by a direct-writing 3D printer, the printing speed is 10mm/s, and the number of printing layers is 5; then the hollow microsphere ceramic slurry with 160-200 meshes is replaced, printing is continued on the basis of the blank, the printing speed is 10mm/s, and the number of printing layers is 5; and repeating the printing process (the printing speed is 10mm/s and the printing layer number is 5) by using the hollow microsphere ceramic slurry with 120-160 meshes and 100-120 meshes to obtain a final ceramic blank.
(4) And discharging the glue from the ceramic blank dried for 9 hours at the temperature of 45 ℃ for 1 hour at the temperature of 600 ℃, and then sintering for 4 hours at the temperature of 1350 ℃, wherein the heating rate of the glue discharging and sintering processes is 4 ℃/min. And cooling along with the furnace after sintering to obtain the porous ceramic with the gradient pore structure framework. The mechanical strength change from bottom layer to top layer of the obtained sample is 4.4 MPa-3.7 MPa, and the thermal conductivity change is 0.37 W.m -1 ·K -1 →0.33W·m -1 ·K -1 。
Example 3
Preparing porous ceramics with a gradient pore structure framework:
(1) The flyash hollow microspheres with the grain diameters of 120-160 meshes (97-125 mu m), 160-200 meshes (75-97 mu m), 200-300 meshes (54-75 mu m) and 300-500 meshes (25-54 mu m) are obtained by screening through a standard sieve, and the flyash hollow microspheres, the ceramic powder, the deionized water, the ammonium citrate dispersing agent and the protein powder with the mass ratio of 27:30:35:0.6:5 are mixed and then are rotated and stirred uniformly to obtain the multi-type ceramic slurry with the hollow microspheres with different grain diameters.
(2) Pouring each ceramic slurry into a centrifugal tank with an opening at the top, and then placing the ceramic slurry into a vacuum defoaming machine (the set vacuum degree is 0.4kPa, and the defoaming time is 5 minutes) to perform defoaming treatment on the ceramic slurry.
(3) After defoaming is finished, firstly, hollow microsphere ceramic slurry with 300-500 meshes is selected and printed by a direct-writing 3D printer, the printing speed is 5mm/s, and the number of printing layers is 5; then the hollow microsphere ceramic slurry with 200-300 meshes is replaced to continue printing on the basis of the blank, the printing speed is 5mm/s, and the number of printing layers is 4; and repeating the printing process (the printing speed is 10mm/s, and the printing layers are 3 layers and 2 layers respectively) by using 160-200 meshes and 120-160 meshes of hollow microsphere ceramic slurry to obtain a final ceramic blank.
(4) And discharging the glue from the ceramic blank dried for 8 hours at the temperature of 55 ℃ for 1 hour at the temperature of 600 ℃, and then sintering for 4 hours at the temperature of 1550 ℃, wherein the heating rate of the glue discharging and sintering processes is 4 ℃/min. And cooling along with the furnace after sintering to obtain the porous ceramic with the gradient pore structure framework. The mechanical strength change from bottom layer to top layer of the obtained sample is 4.7 MPa-3.9 MPa, and the thermal conductivity change is 0.37 W.m -1 ·K -1 →0.34W·m -1 ·K -1 。
Example 4
Preparing porous ceramics with a gradient pore structure framework:
(1) The flyash hollow microspheres with the grain diameters 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) are obtained by screening through a standard sieve, and the flyash hollow microspheres, the ceramic powder, the deionized water, the ammonium citrate dispersing agent and the protein powder with the mass ratio of 32:28:38:0.9:4 are mixed and then are rotated and stirred uniformly to obtain the multi-type ceramic slurry with the hollow microspheres with different grain diameters.
(2) Pouring each ceramic slurry into a centrifugal tank with an opening at the top, and then placing the ceramic slurry into a vacuum defoaming machine (the set vacuum degree is 0.4kPa, and the defoaming time is 10 minutes) to perform defoaming treatment on the ceramic slurry.
(3) After defoaming is finished, firstly, 160-200 meshes of hollow microsphere ceramic slurry is selected and printed by a direct-writing type 3D printer, the printing speed is 15mm/s, and the number of printing layers is 2; then the hollow microsphere ceramic slurry with 120-160 meshes is replaced, printing is continued on the basis of the blank, the printing speed is 15mm/s, and the number of printing layers is 3; and repeating the printing process (the printing speed is 15mm/s, and the printing layers are 4 layers and 5 layers respectively) by using 100-120 meshes and 80-100 meshes of hollow microsphere ceramic slurry to obtain a final ceramic blank.
(4) And discharging the glue from the ceramic blank dried for 10 hours at 50 ℃ for 1 hour at 600 ℃, and then sintering for 4 hours at 1250 ℃, wherein the heating rate of the glue discharging and sintering processes is 2 ℃/min. And cooling along with the furnace after sintering to obtain the porous ceramic with the gradient pore structure framework. The mechanical strength change from bottom layer to top layer of the sample is 4.2 MPa-3.5 MPa, and the thermal conductivity change is 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, hollow microspheres with different particle size ranges are obtained by screening by using a standard sieve as a raw material, and the porous ceramic with the gradient pore structure skeleton is prepared by controlling the printing sequence, so that the rapid regulation and control of the pore structure inside the porous ceramic three-dimensional skeleton is realized, and the method is simple and effective, and ceramic products with complex shapes can be prepared. Has important significance for 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, is favorable for the ultra-light weight of the porous ceramic, and has important research and application values.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (4)
1. The 3D printing forming method of the porous ceramic with the gradient pore structure framework is characterized by comprising the following steps of:
(1) Mixing hollow microspheres with different particle size distributions with ceramic powder, water, a dispersing agent and protein powder respectively 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 respectively;
(3) 3D printing the ceramic slurry with the hollow microspheres with different particle sizes according to a certain hollow microsphere particle size sequence, drying, discharging glue, sintering the obtained blank, and cooling along with a furnace to obtain the porous ceramic with the gradient pore structure skeleton;
the hollow microsphere is fly ash hollow microsphere and Al 2 O 3 Hollow microsphere, siO 2 Hollow microspheres and ZrO 2 One or more of the hollow microspheres;
the ceramic powder is aluminum silicate powder and Al 2 O 3 、SiO 2 And ZrO(s) 2 The particle size of the powder is 1-10 mu m;
the mass ratio of the hollow microspheres to the ceramic powder, water, the dispersing agent and the protein powder is 27-33:27-33:34-40:0.3-0.9:2.4-7.2;
the 3D printing mode in the step (3) is direct-writing printing, and the printing speed is 5-30 mm/s;
the temperature of the adhesive discharge is 600 ℃ and the time is 1-2 h; the sintering temperature is 1250-1550 ℃ and the sintering time is 2-6 h.
2. The 3D printing forming method according to claim 1, wherein the vacuum degree at the time of the defoaming treatment is 0.6kPa or less and the defoaming time is 5 to 15min.
3. The 3D printing forming method of claim 1, wherein the temperature rise rate of the paste discharging and sintering is 2-5 ℃/min.
4. A porous ceramic having a gradient pore structure skeleton prepared by the 3D printing forming method of any one of claims 1 to 3.
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