CN113754412A - Preparation method of high-strength energy-absorbing ceramic-polymer composite structure and product thereof - Google Patents
Preparation method of high-strength energy-absorbing ceramic-polymer composite structure and product thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-strength energy-absorbing ceramic-polymer composite structure and a product thereof, and belongs to the technical field of 3D printing and forming. The method comprises the steps of finishing drawing of a three-dimensional structure model of a ceramic lattice framework through drawing software; preparing ceramic slurry required by printing a three-dimensional structure of a ceramic dot matrix framework, and 3D printing the three-dimensional structure of the ceramic dot matrix framework; and pouring the polymer into a mold with a three-dimensional structure of the ceramic lattice framework, standing and drying to obtain the ceramic-polymer composite structure. According to the invention, the ceramic lattice framework is prepared by using a ceramic material 3D printing technology, the toughness of the ceramic material is improved by coating the ceramic lattice framework with the polymer, and the finally prepared ceramic-polymer composite structure has ultrahigh energy absorption characteristic and can be used under a high-speed impact condition.
Description
Technical Field
The invention relates to the technical field of 3D printing and forming, in particular to a preparation method of a high-strength energy-absorbing ceramic-polymer composite structure and a product thereof.
Background
With the rapid development of advanced technical industries such as aviation, aerospace, ships and warships, higher requirements are put forward on light-weight bearing energy-absorbing materials and structures. Therefore, in order to satisfy the above requirements, it is necessary to develop lightweight materials and members having high strength and high energy absorption, and to satisfy the mechanical requirements thereof in severe environments. The ceramic material has the characteristics of high hardness, high bearing capacity and the like, and plays an indispensable role in modern industry. However, ceramic materials are brittle and sensitive to defects, and are easily damaged catastrophically under an external load, which severely restricts the application of the ceramic materials.
At present, patent number CN106630961A discloses a high-strength building composite ceramic material and a preparation method thereof, the patent adopts red mud, n-butyl zirconium, wollastonite, pottery clay, industrial waste, polybutadiene epoxy resin, flint clay and dibutyl phthalate to be effectively proportioned, so that the ceramic has higher strength, good compactness and good oxidation and corrosion resistance. However, the ceramic material is far from sufficient in high strength, and the ceramic material needs to have the characteristic of high energy absorption at the same time to meet the requirements of advanced technical industries such as aviation, aerospace, ships and the like. Therefore, it is required to develop a ceramic-polymer composite structure having high strength and good energy absorption effect.
Disclosure of Invention
The invention aims to provide a preparation method of a high-strength energy-absorbing ceramic-polymer composite structure and a product thereof, aiming at solving the problems of high brittleness, sensitive defects, easy damage under external load and the like of ceramic materials.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a preparation method of a high-strength energy-absorbing ceramic-polymer composite structure, which specifically comprises the following steps:
(1) structural design of the ceramic lattice framework: drawing a three-dimensional structure model of the ceramic dot matrix framework by Solidworks or Rhino software, and importing the three-dimensional structure model of the ceramic dot matrix framework in stl format into 10dim software to slice the model to obtain a tdp file which can be identified by a printer;
(2)3D printing of a ceramic lattice framework: preparing ceramic slurry required by printing a three-dimensional structure of the ceramic lattice framework, guiding the tdp file obtained in the step (1) into a printer, and setting the ultraviolet power to be 6000-15000 mu W/cm2The single-layer exposure time is 3-10 s. Removing the support material on the green body after printing, washing with alcohol to obtain a green body with a three-dimensional structure of the ceramic lattice framework, and drying, degreasing and sintering the green body to obtain a 3D printed three-dimensional structure of the ceramic lattice framework;
(3) preparation of ceramic-polymer composite structure: and pouring the polymer into a mold with a three-dimensional structure of the ceramic lattice framework, standing and drying to obtain the high-strength energy-absorbing ceramic-polymer composite structure.
Further, the ceramic lattice framework structure in the step (1) comprises truss type lattice frameworks shown in fig. 1(a) to (d) and extremely small curved surface type lattice frameworks shown in fig. 1(e) to (h); the relative density of the cells of the ceramic lattice framework is 10-60%.
Further, in the step (1), the ceramic lattice framework comprises an extremely small curved surface type lattice framework and a truss type lattice framework, the length, the width and the height of the extremely small curved surface type lattice framework are equal, and the length and the width of the truss type lattice framework have no equal requirements.
Further, all the trusses in the single truss type lattice framework cell in the step (1) are equal in diameter, and the wall thickness of the single extremely-small curved surface type lattice framework cell is kept consistent.
Furthermore, the length of the cells of the ceramic lattice framework is 1-30 mm, the width is 1-30 mm, and the number of the cells in the length direction, the width direction and the height direction is 1-10.
Furthermore, the included angle between the diagonal line of the cell element body of the truss lattice skeleton and the projection of the cell element body on the bottom surface is 20-75 degrees, and the size in the height direction satisfies the formula (1):
wherein H is the height of the cell of the truss-like ceramic lattice framework, A, B is the length and width of the cell respectively, and theta is the included angle between the body diagonal of the cell and the projection of the body diagonal on the bottom surface.
Further, the raw materials of the ceramic slurry in the step (2) comprise: ceramic powder, a dispersant, photosensitive resin, a photoinitiator and a sintering aid.
Further, the ceramic powder is any one of alumina, zirconia, silica, silicon carbide, silicon nitride and aluminum nitride, and the dispersant is KOS110 dispersant or Lubo-run hyperdispersant 17000; the photoinitiator is a TPO photoinitiator, and the sintering aid is one or more of titanium dioxide, yttrium oxide and magnesium oxide. Preparing ceramic slurry: the volume content of the ceramic powder is 50 vol.%, the content of the photosensitive resin is 50 vol.%, the addition amount of the dispersing agent KOS110 is 2 wt.% of the use amount of the ceramic powder, the addition amount of the photoinitiator TPO is 1 wt.% of the use amount of the photosensitive resin, the use amount of the sintering aid titanium dioxide is 3 wt.% of the use amount of the ceramic powder, the use amount of the magnesium oxide is 1 wt.% of the use amount of the ceramic powder, and the ceramic slurry is obtained after ball milling for 12 hours.
Further, the alcohol washing in the step (2) is carried out by absolute ethyl alcohol washing, the drying is carried out for 10 hours at room temperature, the grease discharging is carried out for 1-2 hours at 500-600 ℃, and the sintering is carried out for 1-2 hours at 1400-1800 ℃.
Further, the 3D printing in step (2) is one of a stereolithography technique and a digital light processing technique.
Further, in the step (3), the polymer is any one of polymethyl methacrylate, epoxy resin and modified polyurea elastomer, and the modified polyurea elastomer is preferably phenolic aldehyde modified polyurea elastomer.
The invention also provides a high-strength energy-absorbing ceramic-polymer composite structure prepared by the preparation method of the high-strength energy-absorbing ceramic-polymer composite structure.
The invention discloses the following technical effects:
(1) according to the invention, the configuration regulation of the truss type ceramic lattice framework can be realized by designing the length, width and angle of the ceramic lattice framework cell element so as to adapt to working spaces with different sizes. The calculated value of the height thereof satisfies formula (1):
wherein H is the height of the cell of the truss-like ceramic lattice framework, A, B is the length and width of the cell respectively, and theta is the included angle between the body diagonal of the cell and the projection of the body diagonal on the bottom surface.
For example, when the length and the width of the truss type ceramic lattice framework cell element are both 10mm and theta is 20-40 degrees, the height of the cell element can be effectively regulated within the range of 5.15-11.86 mm;
for example, when theta of the truss type ceramic lattice framework cell element is 35 degrees, and the length and the width of the cell element are both 5-30 mm, the height of the cell element can be effectively regulated within the range of 5-30 mm.
The ceramic frameworks with different configurations have different performances such as compression strength, impact strength, energy absorption, strain and the like, the mechanical property of the ceramic framework with the same configuration also changes along with the increase of relative density, and the mechanical property of the ceramic framework with the same configuration also changes along with the change of theta when the relative density is the same. The mechanical properties of the cells with different parameters are different, the working conditions are different, and the design of the overall mechanical properties of the component can be realized through the matching of different cells.
(2) In the invention, different ceramic-polymer composite structures can be obtained by regulating and controlling the configuration, the relative density and the polymer type of the ceramic lattice framework.
(3) In the invention, high-strength ceramic and high-toughness polymer are used as raw materials, a ceramic-polymer composite structure is designed and prepared, and the design of the high-strength and ultrahigh energy-absorbing ceramic-polymer composite structure is realized; the ceramic lattice framework is prepared by using a ceramic material 3D printing technology, and the ceramic lattice framework is coated by a polymer to realize the toughening effect of the ceramic material. The ceramic-polymer composite structure prepared by the invention has ultrahigh energy absorption characteristic and can be used under high-speed impact conditions (such as bulletproof).
(4) The preparation method of the ceramic slurry is simple and easy to operate, and the high-precision molding of various complex structures can be realized by adopting a photocuring 3D printing molding technology, such as a stereolithography molding technology (SLA) and a digital light processing molding technology (DLP).
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 a schematic diagram of different cells of the ceramic lattice framework of the present invention, wherein A, B represents the length and width of a cell, H represents the height of a cell, and θ represents the angle between the diagonal of a truss-like cell and the projection of the truss-like cell on the bottom surface; FIGS. 1(a) - (h) are modified BCC, Octet, Cubic, schwartzP, Gyroid, Diamond and IWP structures, respectively;
FIG. 2 is a pictorial representation of a ceramic-polymer composite structure of example 1 of the present invention;
FIG. 3 is a graph showing the results of mechanical properties of the ceramic-polymer composite structure under dynamic loading in example 1 of the present invention;
FIG. 4 is a pictorial representation of a ceramic-polymer composite structure of example 2 of the present invention;
FIG. 5 is a graph showing the results of mechanical property tests of the ceramic-polymer composite structure under dynamic load in example 2 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 description and examples are intended to be illustrative 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
(1) Designing a ceramic lattice framework structure: a three-dimensional model of the truss-like ceramic lattice skeleton shown in FIG. 1(a) is plotted, wherein the unit cell theta is 40 degrees, the relative density is 25 percent, the length and the width are both 10mm, and the height of the unit cell obtained according to the formula (1) is 11.86 mm. The arrangement of the unit cells in the x, y and z directions is 3 × 3 × 1. And (4) importing the three-dimensional model of the stl-format ceramic lattice framework into 10dim software to be sliced to obtain a tdp file, wherein the slice thickness is 100 micrometers.
(2)3D printing of a ceramic lattice framework:
preparing alumina slurry: wherein the volume content of the alumina ceramic powder is 50 vol.%, the content of the photosensitive resin is 50 vol.%, the addition amount of the dispersing agent KOS110 is 2 wt.% of the dosage of the alumina ceramic powder, the addition amount of the photoinitiator TPO is 1 wt.% of the dosage of the photosensitive resin, the dosage of the sintering aid titanium dioxide is 3 wt.% of the dosage of the alumina ceramic powder, the dosage of the magnesium oxide is 1 wt.% of the dosage of the alumina ceramic powder, and the alumina slurry can be obtained after ball milling for 12 h.
Preparing a green body of the three-dimensional structure of the ceramic lattice framework: and (3) importing the tdp file obtained in the step (1) into a printer. Setting the ultraviolet power at 12000 mu W/cm2The monolayer exposure time was 6 s. And removing the support material on the green body after printing is finished, and cleaning the green body by using absolute ethyl alcohol to obtain the green body with the three-dimensional structure of the ceramic lattice framework.
Sintering the ceramic lattice framework: and drying the green body at room temperature for 10h, degreasing at 600 ℃ for 2h, and sintering at 1400 ℃ for 2h to obtain the 3D printed ceramic lattice framework.
(3) Preparation of ceramic-polymer composite structure: and (3) placing the obtained ceramic lattice framework in a square mould, pouring the liquid phenolic aldehyde modified polyurea elastomer and waiting for gelation to obtain the ceramic-polymer composite structure shown in figure 2.
The mechanical properties of the ceramic-polymer composite structure obtained above at an impact velocity of 11.3m/s were measured by a split Hopkinson pressure bar, and the test results are shown in FIG. 3, wherein the specific strength of the composite material is 124.69N m/g, and the specific energy absorption is 36.18J/g.
Example 2
(1) Designing a ceramic lattice framework structure: drawing a three-dimensional model of the truss-like ceramic lattice framework shown in fig. 1 (a). Wherein the unit cell theta is 40 DEG, the relative density is 25%, the length and the width are both 10mm, and the height of the unit cell obtained according to the formula (1) is 11.86 mm. The arrangement of the unit cells in the x, y and z directions is 3 × 3 × 1. And (4) importing the three-dimensional model of the stl-format ceramic lattice framework into 10dim software to be sliced to obtain a tdp file, wherein the slice thickness is 100 micrometers.
(2)3D printing of a ceramic lattice framework:
preparing alumina slurry: wherein the volume content of the alumina ceramic powder is 50 vol.%, the content of the photosensitive resin is 50 vol.%, the addition amount of the dispersing agent KOS110 is 2 wt.% of the dosage of the alumina ceramic powder, the addition amount of the photoinitiator TPO is 1 wt.% of the dosage of the photosensitive resin, the dosage of the sintering aid titanium dioxide is 3 wt.% of the dosage of the alumina ceramic powder, the dosage of the magnesium oxide is 1 wt.% of the dosage of the alumina ceramic powder, and the alumina slurry can be obtained after ball milling for 12 h.
Preparing a green body of the three-dimensional structure of the ceramic lattice framework: and (3) importing the tdp file obtained in the step (1) into a printer. Setting the power of the ultraviolet light to 13000 mu W/cm2The monolayer exposure time was 3 s. And removing the support material on the green body after printing is finished, and cleaning the green body by using absolute ethyl alcohol to obtain the green body with the three-dimensional structure of the ceramic lattice framework.
Sintering the ceramic lattice framework: and drying the green body at room temperature for 10h, degreasing at 600 ℃ for 2h, and sintering at 1800 ℃ for 2h to obtain the 3D printed ceramic lattice framework.
(3) Preparation of ceramic-polymer composite structure: and (3) placing the obtained ceramic lattice framework in a square mould, pouring the liquid phenolic aldehyde modified polyurea elastomer and waiting for gelation to obtain the ceramic-polymer composite structure shown in figure 4.
The mechanical properties of the ceramic-polymer composite structure obtained above at an impact velocity of 10.8m/s were measured by a split Hopkinson pressure bar, and the test results are shown in FIG. 5, wherein the specific strength of the composite material is 178.01N m/g, and the specific energy absorption is 45.87J/g.
Example 3
The difference from example 1 is that alumina is replaced by zirconia and the phenolic-modified polyurea elastomer is replaced by polymethyl methacrylate.
Example 4
The difference from example 1 is that aluminum oxide was replaced with silicon carbide and the UV power was set to 12000. mu.W/cm2The single-layer curing thickness is 50 mu m, and the single-layer exposure time is 10 s; the sintering condition is changed to 1700 ℃ vacuum sintering for 2 h.
Example 5
The same as example 1 except that the alumina was replaced by silicon nitride, the green body was dried at room temperature for 10 hours, degreased at 500 ℃ for 1 hour, and vacuum-sintered at 1700 ℃ for 1 hour.
Comparative example 1
The difference from example 1 is that the volume content of alumina ceramic powder is 30 vol.%, the content of photosensitive resin is 70 vol.%, the addition amount of dispersant KOS110 is 1 wt.% of the usage amount of alumina ceramic powder, the addition amount of photoinitiator TPO is 2 wt.% of the usage amount of photosensitive resin, the usage amount of sintering aid titanium dioxide is 3 wt.% of the usage amount of alumina ceramic powder, and the usage amount of magnesium oxide is 2 wt.% of the usage amount of alumina ceramic powder.
Comparative example 2
The difference from example 1 is that the UV power is set to 9000. mu.W/cm2The single-layer curing thickness is 75 mu m, and the single-layer exposure time is 4 s; during the sintering process of the ceramic lattice framework, the green body is dried for 10 hours at room temperature, degreased for 1 hour at 450 ℃ and sintered for 4 hours at 1300 ℃.
Comparative example 3
The difference from example 1 is that no polymer bonding process is performed, and only a 3D printed ceramic lattice skeleton is obtained.
The mechanical properties of the composite structures of examples 1 to 5 and comparative examples 1 to 3 and the pure ceramic lattice framework at an impact speed of 10.8m/s were measured by using a split hopkinson pressure bar, wherein the specific strength is strength/density, and the specific energy absorption is total energy absorption/density. The test results are shown in Table 1.
TABLE 1
| Item | Specific strength (N m/g) | Energy absorption ratio (J/g) |
| Example 1 | 124.69 | 36.18 |
| Example 2 | 178.01 | 45.87 |
| Example 3 | 108.55 | 30.25 |
| Example 4 | 151.73 | 35.64 |
| Example 5 | 130.25 | 33.26 |
| Comparative example 1 | 95.62 | 20.15 |
| Comparative example 2 | 110.71 | 28.37 |
| Comparative example 3 | 125.23 | 9.08 |
As can be seen from Table 1, the ceramic-polymer composite structures of examples 1 to 5 are superior to comparative examples in specific strength and specific energy absorption, the specific strength can reach 178.01 N.m/g, and the specific energy absorption can reach 45.87J/g. According to the invention, the ceramic lattice framework is prepared by using a ceramic material 3D printing technology, the ceramic lattice framework is coated by the polymer, the toughening effect of the ceramic material is realized, and the finally prepared ceramic-polymer composite structure has the characteristics of high strength and ultrahigh energy absorption.
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 (10)
1. A preparation method of a high-strength energy-absorbing ceramic-polymer composite structure is characterized by comprising the following steps:
(1) structural design of the ceramic lattice framework: drawing a three-dimensional structure model of the ceramic lattice framework by drawing software;
(2)3D printing of a ceramic lattice framework: preparing ceramic slurry required by printing a three-dimensional structure of a ceramic dot matrix framework, 3D printing the three-dimensional structure of the ceramic dot matrix framework, removing a support material on a green body after printing, washing with alcohol to obtain the green body of the three-dimensional structure of the ceramic dot matrix framework, and drying, degreasing and sintering the green body to obtain the 3D printed three-dimensional structure of the ceramic dot matrix framework;
(3) preparation of ceramic-polymer composite structure: and pouring the polymer into a mold with a three-dimensional structure of the ceramic lattice framework, standing and drying to obtain the high-strength energy-absorbing ceramic-polymer composite structure.
2. The method for preparing a high-strength energy-absorbing ceramic-polymer composite structure according to claim 1, wherein the ceramic lattice framework in the step (1) comprises a very small curved surface type lattice framework and a truss type lattice framework, the very small curved surface type lattice framework has equal length, width and height, and the truss type lattice framework has no equal requirement on length and width.
3. The method of claim 2, wherein the ceramic lattice framework has a length of 1-30 mm and a width of 1-30 mm, and the number of cells in the length, width and height directions is 1-10.
4. The method for preparing a high-strength energy-absorbing ceramic-polymer composite structure according to claim 2, wherein an included angle between a diagonal line of a cell body of the lattice-like truss framework and a projection of the diagonal line on a bottom surface is 20-75 degrees, and the dimension in the height direction satisfies formula (1):
wherein H is the height of the cell of the truss-like ceramic lattice framework, A, B is the length and width of the cell respectively, and theta is the included angle between the body diagonal of the cell and the projection of the body diagonal on the bottom surface.
5. The method for preparing a high-strength energy-absorbing ceramic-polymer composite structure according to claim 1, wherein the raw materials of the ceramic slurry in the step (2) comprise: ceramic powder, a dispersant, photosensitive resin, a photoinitiator and a sintering aid.
6. The method for preparing a high-strength energy-absorbing ceramic-polymer composite structure according to claim 5, wherein the ceramic powder is any one of alumina, zirconia, silica, silicon carbide, silicon nitride and aluminum nitride, the dispersant is KOS110 dispersant or Lubo super dispersant 17000, the photoinitiator is TPO photoinitiator, and the sintering aid is one or more of titanium dioxide, yttrium oxide and magnesium oxide.
7. The method for preparing a high-strength energy-absorbing ceramic-polymer composite structure according to claim 1, wherein the alcohol washing in the step (2) is performed by absolute ethyl alcohol, the drying is performed at room temperature for 10 hours, the grease discharging is performed at 500-600 ℃ for 1-2 hours, and the sintering is performed at 1400-1800 ℃ for 1-2 hours.
8. The method of claim 1, wherein the 3D printing in step (2) is one of stereolithography and digital light processing.
9. The method for preparing a high-energy-absorption ceramic-polymer composite structure according to claim 1, wherein the polymer in the step (3) is any one of polymethyl methacrylate, epoxy resin and modified polyurea elastomer.
10. A high-strength energy-absorbing ceramic-polymer composite structure prepared by the preparation method of the high-strength energy-absorbing ceramic-polymer composite structure according to any one of claims 1 to 9.
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| CN202111079968.4A CN113754412A (en) | 2021-09-15 | 2021-09-15 | Preparation method of high-strength energy-absorbing ceramic-polymer composite structure and product thereof |
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