CN115161508A - Preparation method of designable metal/ceramic two-phase three-dimensional communication protective material and product thereof - Google Patents
Preparation method of designable metal/ceramic two-phase three-dimensional communication protective material and product thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 50
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 46
- 239000002184 metal Substances 0.000 title claims abstract description 46
- 230000001681 protective effect Effects 0.000 title claims abstract description 41
- 238000004891 communication Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims description 16
- 238000000034 method Methods 0.000 claims abstract description 12
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- 238000005245 sintering Methods 0.000 claims description 24
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- 238000010146 3D printing Methods 0.000 claims description 13
- 238000005457 optimization Methods 0.000 claims description 10
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Abstract
The invention discloses a method for preparing a designable metal/ceramic two-phase three-dimensional communication protective material and a product thereof, belonging to the technical field of protective materials.
Description
Technical Field
The invention relates to the technical field of protective materials, in particular to a preparation method of a designable metal/ceramic two-phase three-dimensional communicated protective material and a product thereof.
Background
The purpose of the protective material is to consume the kinetic energy of the projectile and reduce the killing power of the projectile, thereby achieving the purpose of protecting the fighter. The traditional protective material is mostly formed by stacking ceramic and metal sheets in a layered manner. The ceramic layer on the surface of the protective material can effectively upset and damage the bullet and weaken the killing force of the bullet; the broken ceramic can further dissipate the kinetic energy of the bullet; the metal back plate absorbs the remaining energy of the bullet by its plastic deformation. However, the traditional layered protective material has the problems of discontinuous stress transmission, incapability of resisting continuous damage, easiness in splashing of ceramic materials and the like. With the increasing of weapon killing power, the protection performance of the protection material is required to be higher. In addition, the mechanical properties of the protective material are required to be different at different positions, which is an important challenge for the designability of the mechanical properties of the protective material. Therefore, the development of a designable metal/ceramic two-phase three-dimensional communication protective material with high strength, good energy absorption effect and multiple-strike resistance is needed.
Disclosure of Invention
The invention aims to provide a preparation method of a designable metal/ceramic two-phase three-dimensional communication protective material and a product thereof, aiming at solving the problems that the protective material has insufficient protective performance, can not resist multiple times of striking, can not design the mechanical property of the material and the like.
In order to achieve the purpose, the invention provides the following scheme:
a preparation method of a designable metal/ceramic two-phase three-dimensional communication protective material comprises the following steps:
designing a three-dimensional structure of a ceramic framework, preparing the ceramic framework by using a 3D printing technology, and filling molten metal into the space around the ceramic framework by using a vacuum infiltration technology.
Further, the preparation method specifically comprises the following steps:
(1) Designing a three-dimensional structure of the ceramic framework: drawing a ceramic framework three-dimensional model, slicing the stl-format ceramic framework three-dimensional model to obtain a tdp file, preferably finishing drawing the ceramic framework three-dimensional model through Solidworks, rhino and other software, and importing the stl-format ceramic framework three-dimensional model into 10dim software to slice the model to obtain the tdp file which can be identified by a printer;
(2) 3D printing of a ceramic framework: preparing ceramic slurry required by printing a ceramic framework, importing the tdp file into a printer for 3D printing, and setting the ultraviolet light power to be 5500-18000 mu W/cm 2 The single-layer exposure time is 2-12 s, after printing is completed, the supporting material on the green body is removed, alcohol washing is carried out, the green body of the ceramic framework is obtained, and drying, grease discharging and sintering treatment are carried out on the green body, so that the 3D printed ceramic framework is obtained;
(3) The preparation of the metal/ceramic two-phase three-dimensional communication protective material can be designed as follows: and embedding the ceramic framework into metal powder, sintering in vacuum, melting the metal powder to fill the space where the ceramic framework is located, and thus obtaining the designable metal/ceramic two-phase three-dimensional communication protective material.
Further, the ceramic skeleton cell elements of the ceramic skeleton three-dimensional model in the step (1) comprise a lattice structure, a minimum curved surface structure and a topology optimization structure thereof, and the cell element configurations and relative densities at different positions of the ceramic skeleton have no equal requirements.
Further, the relative density of the ceramic framework cell elements of the three-dimensional ceramic framework model in the step (1) is 5-75%.
Further, the length, the width and the height of the ceramic framework cell element of the three-dimensional ceramic framework model in the step (1) are 1-30 mm, and no equal requirements exist.
Further, the 3D printing in the step (2) is a photocuring 3D printing molding technology, which may be one of a stereolithography molding technology and a digital light processing molding technology.
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;
the dispersant is KOS110 dispersant or Luobutren hyperdispersant 17000;
the photoinitiator is TPO photoinitiator;
the sintering aid is one or more of titanium dioxide, yttrium oxide and magnesium oxide;
30-60 vol.% of ceramic powder, 40-70 vol.% of photosensitive resin, 1-5 wt.% of dispersant, 0.5-2 wt.% of photoinitiator, 0.5-5 wt.% of sintering aid and 0.5-3 wt.% of ceramic powder when the sintering aid is magnesium oxide.
The preparation method of the ceramic powder comprises the following steps: the raw materials are mixed according to the proportion and then ball-milled for 6-40 h to obtain ceramic slurry.
Further, the alcohol washing in the step (2) is washing with absolute ethyl alcohol, and the drying is drying at room temperature for 5 hours.
Further, the grease discharging temperature in the step (2) is 450-650 ℃, and the grease discharging time is 0.5-4 h; the sintering temperature is 1400-1800 ℃, and the sintering time is 0.5-4 h.
Further, the vacuum infiltration temperature in the step (3) is 500-1800 ℃.
The designable metal/ceramic two-phase three-dimensional communication protective material prepared by the preparation method.
The invention discloses the following technical effects:
(1) In the invention, the design and regulation of the mechanical property of the ceramic framework can be realized by designing the configuration, the size and the relative density of the ceramic framework cell element.
(2) In the invention, the designable metal/ceramic two-phase three-dimensional communication protective material with different mechanical property designs can be obtained by regulating and controlling the type of the metal powder.
(3) The invention takes high-strength ceramic and high-plasticity metal as raw materials, designs and prepares a designable metal/ceramic two-phase three-dimensional communication protective material with high strength, high energy absorption, good stress transmission continuity and multiple strike resistance, which is characterized in that: designing a three-dimensional structure of a ceramic framework; preparing a ceramic framework by using a ceramic material 3D printing technology; the molten metal is filled into the space around the ceramic framework by a vacuum infiltration technology, so that the preparation of the designable metal/ceramic two-phase three-dimensional communication protective material is realized. The designable metal/ceramic biphase three-dimensional communication protective material prepared by the invention has the characteristics of high strength and high energy absorption, can resist multiple times of striking, and can be widely applied to body armor, armored vehicles and aircrafts requiring armor protection.
(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 required in the embodiments will be briefly described below, 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 that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a metal/gradient ceramic two-phase three-dimensional connected protective material in example 1 of the present invention;
FIG. 2 is a schematic structural diagram of a metal/topologically optimized ceramic two-phase three-dimensional connected protective material in example 2 of the present invention;
FIG. 3 is a physical diagram of the gradient ceramic skeleton of comparative example 1 based on octahedral truss configuration design;
FIG. 4 is a graph of the results of the mechanical properties test of the octahedral truss configuration-based gradient ceramic framework designed in comparative example 1 under static compressive load;
FIG. 5 is a diagram of a ceramic skeleton topologically optimized based on an octahedral truss configuration in comparative example 2 of the present invention;
fig. 6 is a mechanical property test chart of the octahedral truss configuration based topological optimization ceramic framework under static compression load in comparative example 2 of the 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 intervening value, to the extent 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.
The room temperature in the examples of the present invention means 25. + -. 1 ℃.
The ceramic framework cell element of the ceramic framework three-dimensional model in the embodiment of the invention comprises a lattice structure, a tiny curved surface structure and a topology optimization structure thereof, and the cell element configuration and the relative density of different positions of the ceramic framework have no equal requirements.
Example 1
(1) Designing a three-dimensional model of a gradient ceramic framework:
drawing a gradient ceramic skeleton three-dimensional model with a cell structure of an octahedral truss, wherein the unit cell size is 7.5 multiplied by 7.5mm 3 The arrangement in the x, y and z directions is 4 × 4 × 4. The overall relative density of the structure was 40%, and the relative densities of each layer were 55%,45%,35% and 25%, respectively. And (4) importing the stl format three-dimensional model of the ceramic skeleton into 10dim software to be sliced to obtain a tdp file, wherein the slice thickness is 100 micrometers.
(2) 3D printing of a gradient ceramic framework:
preparing alumina slurry: wherein the volume content of the alumina ceramic powder is 55vol%, the content of the photosensitive resin is 45vol%, the addition amount of the dispersing agent KOS110 is 4wt% of the dosage of the alumina ceramic powder, the addition amount of the photoinitiator TPO is 2wt% of the dosage of the photosensitive resin, the dosage of the sintering aid titanium dioxide is 0.5wt% of the dosage of the alumina ceramic powder, the dosage of the magnesium oxide is 2.5wt% of the dosage of the alumina ceramic powder, and the alumina slurry can be obtained after ball milling for 24 hours.
Preparing a green body of the gradient ceramic framework: and (3) importing the tdp file obtained in the step (1) into a printer. Setting the ultraviolet power at 10000 muW/cm 2 The monolayer exposure time was 7s. 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 of the gradient ceramic framework.
Sintering a gradient ceramic framework: and drying the green body at room temperature for 5h, discharging grease at 450 ℃ for 1h, and sintering at 1550 ℃ for 4h to obtain the 3D printed gradient ceramic skeleton.
(3) Preparing a metal/gradient ceramic two-phase three-dimensional communicated protective material:
embedding the obtained gradient ceramic framework into AlSi10Mg aluminum alloy powder, and placing the powder in a vacuum sintering furnace at 800 ℃ to melt metal powder so as to fill the space where the gradient ceramic framework is located, thereby obtaining the designable metal/gradient ceramic two-phase three-dimensional communication protective material shown in figure 1.
And testing the mechanical property of the metal/gradient ceramic two-phase three-dimensional communicated protective material under the static load by using a universal mechanical testing machine. The strength of the metal/gradient ceramic two-phase three-dimensional communication protective material is 209.89MPa, and the energy absorbed in the compression process is 61.72MJ/m 3 。
And testing the mechanical property of the metal/gradient ceramic two-phase three-dimensional communicated protective material at the impact speed of 12 +/-0.5 m/s by using a separated Hopkinson pressure bar. The dynamic strength of the metal/gradient ceramic two-phase three-dimensional communicated protective material is 162.57MPa, and the energy absorbed in the compression process is 3.75MJ/m 3 And the high-speed impact-resistant material can still maintain excellent mechanical properties and high structural integrity after being subjected to 5 times of high-speed impact.
Example 2
(1) Designing a three-dimensional model of a topological optimization ceramic framework:
drawing a ceramic skeleton three-dimensional model based on octahedral truss structure topological optimization, wherein the relative density is 40 percent, and the unit cell size is 7.5 multiplied by 7.5mm 3 The arrangement in the x, y and z directions is 4 × 4 × 4. And (4) importing the stl format three-dimensional model of the topology optimization ceramic skeleton into 10dim software to be sliced to obtain a tdp file, wherein the slice thickness is 75 micrometers.
(2) 3D printing a topologically optimized ceramic skeleton:
preparing alumina slurry: wherein the volume content of the alumina ceramic powder is 50vol%, the content of the photosensitive resin is 50vol%, the addition amount of the Lu Borun hyper-dispersant 17000 is 3wt% of the dosage of the alumina ceramic powder, the addition amount of the photoinitiator TPO is 1wt% of the dosage of the photosensitive resin, the dosage of the sintering aid titanium dioxide is 3wt% of the dosage of the alumina ceramic powder, the dosage of the magnesium oxide is 0.5wt% of the dosage of the alumina ceramic powder, and the alumina slurry can be obtained after ball milling for 12 hours.
Preparing a green body of the topology-optimized ceramic framework: and (3) importing the tdp file obtained in the step (1) into a printer. Setting the ultraviolet power at 8000 mu W/cm 2 The monolayer exposure time was 6s. 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 of the topology-optimized ceramic framework.
Sintering a topological optimized ceramic framework: and drying the green body at room temperature for 5h, degreasing at 550 ℃ for 0.5h, and sintering at 1600 ℃ for 2h to obtain the 3D printed topologically optimized ceramic framework.
(3) Preparing a metal/topology optimization ceramic two-phase three-dimensional communicated protective material:
embedding the obtained topology optimization ceramic framework into AlSi10Mg aluminum alloy powder, placing the powder in a vacuum sintering furnace at 750 ℃ to melt metal powder so as to fill the space where the ceramic framework is located, and obtaining the designable metal/topology optimization ceramic two-phase three-dimensional communication protective material shown in figure 2.
Example 3
The difference from example 1 is that alumina is replaced with zirconia, and the UV power is set to 12000. Mu.W/cm 2 The single-layer curing thickness is 50 mu m, and the single-layer exposure time is 6s; the sintering condition is changed to 1700 ℃ for sintering for 4h.
Comparative example 1
The difference from example 1 is that, without the metal powder bonding process, only the gradient ceramic skeleton of octahedral truss in the 3D printed cell configuration shown in fig. 3 is obtained. The mechanical property test chart of the structure under the static compression load is shown in figure 4, and the figure 4 shows that the strength of the structure under the quasi-static compression load is close to 9.73MPa, and the energy absorbed in the compression process is 0.06MJ/m 3 。
Comparative example 2
The difference from example 2 is that the bonding process of the metal powder is not performed, and only the 3D printed octahedral truss-based topologically optimized ceramic skeleton shown in fig. 5 is obtained. The structure has a mechanical property test chart under a static compression load as shown in the figure6, as can be seen from FIG. 6, the strength of the structure under quasi-static compression load is 7.56MPa, and the energy absorbed in the compression process is 0.06MJ/m 3 。
Mechanical properties of the metal/ceramic two-phase three-dimensional connected protective materials and the pure ceramic frameworks of examples 1 to 3 and comparative examples 1 to 2 at a static state and an impact speed of 12 +/-0.5 m/s were measured by a universal mechanical testing machine and a split Hopkinson pressure bar. The test results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the metal/ceramic two-phase three-dimensional connected protective materials of examples 1-3 have better strength and energy absorption than the comparative example, and the static strength and energy absorption can reach 209.89MPa and 61.72MJ/m 3 The dynamic strength and energy absorption can reach 162.57MPa and 3.75MJ/m 3 And the dynamic impact resistance times can reach 5 times. According to the invention, the ceramic framework is prepared by using a ceramic material 3D printing technology, and the space where the ceramic framework is located is filled with molten metal by using a vacuum infiltration technology, so that the designable metal/ceramic two-phase three-dimensional communication protective material which is high in strength, high in energy absorption and resistant to multiple strikes is finally obtained.
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 designable metal/ceramic two-phase three-dimensional communication protective material is characterized by comprising the following steps:
designing a three-dimensional structure of a ceramic framework, preparing the ceramic framework by using a 3D printing technology, and filling molten metal into the space around the ceramic framework by using a vacuum infiltration technology.
2. The preparation method according to claim 1, comprising the following steps:
(1) Designing a three-dimensional structure of the ceramic framework: drawing a ceramic framework three-dimensional model, and slicing the stl-format ceramic framework three-dimensional model to obtain a tdp file;
(2) 3D printing of a ceramic framework: preparing ceramic slurry required by printing a ceramic framework, guiding the tdp file into a printer, performing 3D printing, removing a support material on a green body after printing is completed, performing alcohol washing to obtain the green body of the ceramic framework, and performing drying, grease discharging and sintering treatment on the green body to obtain the 3D printed ceramic framework;
(3) The preparation of the metal/ceramic two-phase three-dimensional communicated protective material can be designed as follows: and embedding the ceramic framework into metal powder, and sintering in vacuum to obtain the designable metal/ceramic two-phase three-dimensional communication protective material.
3. The method according to claim 2, wherein the ceramic skeleton cells of the three-dimensional ceramic skeleton model in step (1) comprise lattice structures and infinitesimal curved structures and topology optimization structures thereof.
4. The method according to claim 2, wherein the relative density of the ceramic skeleton cells of the three-dimensional model of the ceramic skeleton in step (1) is 5-75%.
5. The method according to claim 2, wherein the length, width and height of the ceramic skeleton cell of the three-dimensional model of the ceramic skeleton in step (1) are 1mm to 30mm, and there is no requirement for them to be equal.
6. The method according to claim 2, wherein the raw materials of the ceramic slurry of step (2) include: ceramic powder, a dispersant, photosensitive resin, a photoinitiator and a sintering aid.
7. The preparation method according to claim 6, wherein the volume content of the ceramic powder is 30-60 vol.%, the content of the photosensitive resin is 40-70 vol.%, the addition amount of the dispersant is 1-5 wt.% of the dosage of the ceramic powder, the addition amount of the photoinitiator is 0.5-2 wt.% of the dosage of the photosensitive resin, and the dosage of the sintering aid is 0.5-5 wt.% of the dosage of the ceramic powder.
8. The preparation method according to claim 2, wherein the temperature for removing the grease in the step (2) is 450-650 ℃, and the time for removing the grease is 0.5-4 h; the sintering temperature is 1400-1800 ℃, and the sintering time is 0.5-4 h.
9. The method according to claim 2, wherein the vacuum infiltration temperature in step (3) is 500 to 1800 ℃.
10. A designable metal/ceramic two-phase three-dimensional interconnected protective material, characterized in that it is prepared by the method of any one of claims 1 to 9.
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| CN115507703A (en) * | 2022-10-14 | 2022-12-23 | 盐城工学院 | Continuous functional gradient ceramic/metal bionic composite armor and preparation method thereof |
| CN115591015A (en) * | 2022-10-25 | 2023-01-13 | 季华实验室（Cn） | Degradable metal/polymer composite bone fracture plate and preparation method thereof |
| CN117540493A (en) * | 2024-01-09 | 2024-02-09 | 天目山实验室 | Protection-bearing integrated optimization design method for aircraft protection structure |
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| CN111302811A (en) * | 2020-03-31 | 2020-06-19 | 徐州瑞缔新材料科技有限公司 | Preparation method of ceramic reinforced metal matrix composite with ceramic framework designed according to requirements |
| CN113172724A (en) * | 2021-03-05 | 2021-07-27 | 南京航空航天大学 | Preparation process of controllable network ceramic/metal composite material |
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| CN111302811A (en) * | 2020-03-31 | 2020-06-19 | 徐州瑞缔新材料科技有限公司 | Preparation method of ceramic reinforced metal matrix composite with ceramic framework designed according to requirements |
| CN113172724A (en) * | 2021-03-05 | 2021-07-27 | 南京航空航天大学 | Preparation process of controllable network ceramic/metal composite material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115507703A (en) * | 2022-10-14 | 2022-12-23 | 盐城工学院 | Continuous functional gradient ceramic/metal bionic composite armor and preparation method thereof |
| CN115507703B (en) * | 2022-10-14 | 2024-03-15 | 盐城工学院 | Continuous functional gradient ceramic/metal bionic composite armor and preparation method thereof |
| CN115591015A (en) * | 2022-10-25 | 2023-01-13 | 季华实验室（Cn） | Degradable metal/polymer composite bone fracture plate and preparation method thereof |
| CN115591015B (en) * | 2022-10-25 | 2024-01-26 | 季华实验室 | Degradable metal/polymer composite bone fracture plate and preparation method thereof |
| CN117540493A (en) * | 2024-01-09 | 2024-02-09 | 天目山实验室 | Protection-bearing integrated optimization design method for aircraft protection structure |
| CN117540493B (en) * | 2024-01-09 | 2024-04-12 | 天目山实验室 | Protection-bearing integrated optimization design method for aircraft protection structure |
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