CN112548100A - Preparation method of bionic oriented ordered laminated composite material - Google Patents

Preparation method of bionic oriented ordered laminated composite material Download PDF

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CN112548100A
CN112548100A CN202011550561.0A CN202011550561A CN112548100A CN 112548100 A CN112548100 A CN 112548100A CN 202011550561 A CN202011550561 A CN 202011550561A CN 112548100 A CN112548100 A CN 112548100A
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composite material
laminated composite
slurry
powder
cooling
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CN112548100B (en
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姚正军
杜文博
束长青
章旗超
张帆
李祥硕
姚孟欣
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D19/00—Casting in, on, or around objects which form part of the product
    • B22D19/16—Casting in, on, or around objects which form part of the product for making compound objects cast of two or more different metals, e.g. for making rolls for rolling mills
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F3/26—Impregnating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

The invention discloses a preparation method of a bionic oriented ordered laminated composite material, which comprises the following steps: step one, preparing frozen casting slurry: the slurry comprises xanthan gum solution, polyvinyl alcohol and powder; the powder is one or a mixture of metal, metal compound and ceramic; uniformly mixing all the components, and removing bubbles to obtain frozen casting slurry; step two, guiding the frozen casting slurry into a mold, and directionally freezing until the surface is completely frozen to obtain solid slurry; step three, putting the solid slurry into a pre-freezing chamber for continuous freezing, and then carrying out freeze drying to obtain an original embryo body; sintering the original blank to obtain a porous framework; placing the melt-leaching material around the porous framework, heating for melt-leaching, and cooling and solidifying at room temperature to obtain a laminated composite material; the melt-leaching material is metal, macromolecule or the mixed material of macromolecule and ceramic. The invention can successfully prepare the bionic laminated material.

Description

Preparation method of bionic oriented ordered laminated composite material
Technical Field
The invention belongs to the field of materials, relates to a composite material, and particularly relates to a preparation method of a bionic oriented ordered laminated composite material.
Background
The requirement of aerospace on high-performance materials is higher and higher, and the high-performance plate material means longer service time and safer service environment. The high strength can reduce the material usage amount and achieve the corresponding mechanical property, and meets the requirement of the country and the industry for light weight. The good toughness improves the work required by the material component for failure and breakage, so that the safety of the material in a service environment can be well ensured.
In addition to the demands for room temperature properties, the modern industry also places stringent demands on high temperature properties. The temperature of the industrial gas turbine and the internal combustion engine can reach 500-600 ℃ after compression. In the petrochemical industry, the temperature of a furnace tube of a hydrogen production heating furnace is as high as 1000 ℃, and the temperature of an air compressor is generally about 400-700 ℃ as an engine of a pearl on a crown. The development of high temperature materials is important to the impact of various industries.
However, related researches show that the composite material with the layered structure has positive effects on the strength and toughness at room temperature and the creep resistance at high temperature. The common preparation methods of the layered composite material comprise vacuum hot pressing, explosive welding, hot charging and rolling and the like, the thickness of the layer is difficult to control to be below 100 mu m at low cost, the equipment requirement is high, and the thinner layer has more interfaces to lose the fracture energy.
Disclosure of Invention
The invention adopts a freezing casting coupling hot dipping process to prepare the layered composite material with the advantages of low equipment requirement, high product controllability, good comprehensive performance and the like, so as to break through the limitation of the traditional layered composite material preparation process.
In order to achieve the above object, the present invention provides a method for preparing a biomimetic oriented ordered laminated composite material, which has the following characteristics: the method comprises the following steps:
step one, preparing frozen casting slurry: the slurry comprises xanthan gum solution, polyvinyl alcohol and powder, wherein the xanthan gum solution and the polyvinyl alcohol are thickening agents; the polyvinyl alcohol accounts for 1 percent of the mass of the powder, and the powder accounts for 20 to 30 percent of the total volume of the slurry; the powder is one or a mixture of metals, metal compounds and ceramics, wherein the metal compounds are compounds which can be decomposed into pure metals at the sintering temperature; uniformly mixing all the components, and removing bubbles to obtain frozen casting slurry;
step two, guiding the frozen casting slurry into a mold, and directionally freezing until the surface is completely frozen to obtain solid slurry; wherein, the directional freezing refers to gradually gradient freezing along a certain direction;
step three, putting the solid slurry into a pre-freezing chamber to continue freezing for at least 5h, then carrying out freeze drying, and taking out after 24h of freeze drying to obtain an original embryo body;
sintering the original blank to obtain a porous framework, wherein the sintering time is 2-5h, and the sintering temperature is less than the melting point of the powder;
placing the melt-leaching material around the porous framework, heating for melt-leaching, wherein the heating temperature is higher than the melting point of the melt-leaching material and lower than the melting point of the framework powder, and cooling and solidifying at room temperature after the heating is finished to obtain the laminated composite material; the melt-leaching material is metal, macromolecule or the mixed material of macromolecule and ceramic.
Further, the invention provides a preparation method of the bionic oriented ordered laminated composite material, which can also have the following characteristics: and in the fifth step, the porous framework is immersed in the melt-leaching material.
Further, the invention provides a preparation method of the bionic oriented ordered laminated composite material, which can also have the following characteristics: wherein the freezing temperature in the third step is-50 ℃.
Further, the invention provides a preparation method of the bionic oriented ordered laminated composite material, which can also have the following characteristics: wherein the powder is TiH2And B4C。
Further, the invention provides a preparation method of the bionic oriented ordered laminated composite material, which can also have the following characteristics: wherein the melt-impregnated material is a resin.
Further, the invention provides a preparation method of the bionic oriented ordered laminated composite material, which can also have the following characteristics: wherein the melt-leaching material is resin and TiB2。
Further, the invention provides a preparation method of the bionic oriented ordered laminated composite material, which can also have the following characteristics: and in the fifth step, heating and melting and soaking by adopting a vacuum sintering furnace.
Further, the invention provides a preparation method of the bionic oriented ordered laminated composite material, which can also have the following characteristics: the second step adopts a refrigerating device for directional refrigeration, wherein the refrigerating device comprises a mold, a metal sheet, a semiconductor refrigerating sheet group, a thermosensitive semiconductor, a temperature controller, a power supply, a metal hollow plate, a cooling pipeline, a cooling liquid storage unit and a cooling and power unit; the mold is a frame body with a circle of closed side walls, and the material of the mold is heat-insulating material; the die is arranged on the metal sheet, and the metal sheet is fixed on the semiconductor refrigerating sheet set; the semiconductor refrigerating sheet set is connected with a power supply, the power supply supplies power to the semiconductor refrigerating sheet set, and the semiconductor refrigerating sheet set is electrified for refrigeration; the temperature controller is connected with the thermosensitive semiconductor and monitors the temperature at the bottom of the die; the temperature controller is also connected with a power supply and controls the refrigerating temperature and the cooling rate of the semiconductor refrigerating sheet set by adjusting the output of the power supply; the semiconductor refrigerating sheet group is fixed on the metal hollow plate; the cooling liquid storage unit is used for storing cooling liquid and is communicated with the metal hollow plate through a cooling pipeline to form a cooling loop so as to provide circulating cooling liquid for the metal hollow plate; the cooling and power unit comprises a cooling device and a power device, is arranged on the cooling pipeline and is used for cooling and conveying cooling liquid;
further, the invention provides a preparation method of the bionic oriented ordered laminated composite material, which can also have the following characteristics: wherein, in the step one, the concentration of the xanthan gum solution is 1.2 g/L.
Further, the invention provides a preparation method of the bionic oriented ordered laminated composite material, which can also have the following characteristics: in the first step, ball milling is adopted to mix the freezing casting slurry.
The invention has the beneficial effects that: the invention provides a near-net forming process for preparing a bionic laminated composite material with a micron scale, which constructs laminated composite materials such as a metal-metal composite material, a metal-macromolecule and the like by designing a structure and a microstructure, reduces the low density of the material and realizes the light weight.
Moreover, the layered material has high fracture toughness due to crack deflection and crack bridging; meanwhile, according to the stress reclassification principle of the composite material, the strength is improved; therefore, the toughness of the material can be improved by utilizing the bionic layered structure.
The method and the device avoid the defects of complex process and high equipment requirement of the traditional processes such as rolling, explosion welding and vacuum hot pressing, and can form the oriented ordered laminated composite material on the micrometer scale. The composite material adopts the freezing casting coupling melting and soaking, firstly utilizes the freezing casting technology to build a layered structure of the layered reinforcing material, utilizes the resin doped with metal or ceramic particles to melt and soak, and finally forms the oriented ordered laminated composite material.
The melt-leaching material in the bionic material is used as a reinforcement, can be a metal material, a high polymer material or a ceramic-doped high polymer material and the like, the porosity in the porous framework is controlled by controlling the proportion of the powder, the content of the laminated reinforcement can be further controlled, the range can be controlled between 30% and 50%, and the laminated width can be prepared between 10 micrometers and 1000 micrometers. The mechanical property of the composite material can be macroscopically regulated and controlled by controlling the content of the reinforcing body and the width of the lamination.
In addition, vacuum infusion may be used to force the infusion material into the skeleton. The melt-leaching process has no influence on the structure of the melt-leaching material and is tightly combined. Finally, the laminated composite material is prepared.
Drawings
FIG. 1 is a schematic view of the structure of a freezer;
FIG. 2 is a view of the structure of a light microscope of the laminated composite material of example 1;
FIG. 3 is a view of the structure of an optical microscope of the laminated composite material of example 2;
FIG. 4 is a view of the structure of an optical microscope of the laminated composite material of example 3;
FIG. 5 is a view of the structure of an optical microscope of the laminated composite material of example 4;
FIG. 6 is a view of the structure of an optical microscope of the laminated composite material of example 5;
FIG. 7 is a view of the structure of an optical microscope of the laminated composite material of example 6;
FIG. 8 is an optical microscope structure and EDS image of the laminated composite material of example 7;
FIG. 9 is an optical microscope structure and EDS image of the laminated composite material of example 8.
Detailed Description
The invention is further described below with reference to the accompanying drawings and specific examples.
The invention provides a preparation method of a bionic oriented ordered laminated composite material, which comprises the following steps:
step one, preparing frozen casting slurry: the slurry comprises xanthan gum solution, polyvinyl alcohol and powder, wherein the xanthan gum solution and the polyvinyl alcohol are thickening agents. The polyvinyl alcohol accounts for 1 percent of the mass of the powder, and the powder accounts for 20 to 30 percent of the total volume of the slurry. The powder is one or a mixture of metals, metal compounds and ceramics, and the metal compounds are compounds which can be decomposed into pure metals at the sintering temperature. The components are uniformly mixed, and bubbles are removed to obtain the frozen casting slurry.
And step two, guiding the frozen casting slurry into a mold, and directionally freezing until the surface is completely frozen to obtain solid slurry. Directional freezing refers to gradual gradient freezing along a certain direction.
The directional freezing was performed using a freezing apparatus as shown in fig. 1. The refrigerating device comprises a mould 1, a metal sheet 2, a semiconductor refrigerating sheet group 3, a thermosensitive semiconductor 4, a temperature controller 5, a power supply 6, a metal hollow plate 7, a cooling pipeline 8, a cooling liquid storage unit 9 and a cooling and power unit 10.
The mold 1 is a frame body with a circle of closed side walls, has no bottom surface and penetrates up and down, and can be in any shape such as a circular ring shape. The die 1 is arranged on the metal sheet 2, and the metal sheet 2 is fixed on the semiconductor refrigerating sheet group 3. Wherein, the mould 1 can be pasted on the metal sheet 2 through the sealing grease, thereby avoiding the leakage of the sizing agent, and the mould 1 is separated from the metal sheet 2 during demoulding.
The semiconductor refrigerating sheet group 3 is connected with a power supply 6, the power supply 6 supplies power to the semiconductor refrigerating sheet group 3, and the semiconductor refrigerating sheet group 3 is electrified for refrigeration. The temperature-sensitive semiconductor 4 is fixed at the bottom of the die 1, and the temperature controller 5 is connected with the temperature-sensitive semiconductor 4 and monitors the temperature at the bottom of the die 1. The temperature controller 5 is also connected with a power supply 6, and controls the refrigerating temperature and the cooling rate of the semiconductor refrigerating sheet set 3 by adjusting the output of the power supply 6.
The semiconductor refrigerating sheet group 3 is fixed on the metal hollow plate 7. The cooling liquid storage unit 9 stores cooling liquid, and the cooling liquid storage unit 9 is communicated with the metal hollow plate 7 through the cooling pipeline 8 to form a cooling loop and provide circulating cooling liquid for the metal hollow plate 7. The cooling and power unit 10 comprises a cooling device and a power device, is arranged on the cooling pipeline 8, and cools and conveys the cooling liquid.
Wherein, the mould 1 is made of heat insulating materials such as polytetrafluoroethylene. The material of the metal foil 2 and the metal hollow plate 7 is preferably copper.
When the semiconductor refrigerating sheet set works, the semiconductor refrigerating sheet set 3 refrigerates and cools slurry in the die 1 through the metal sheet 2 with good heat conducting performance, and the temperature controller 5 controls the power supply 6 according to the temperature monitored by the thermosensitive semiconductor 4, so that the refrigerating temperature and the cooling rate are adjusted. Meanwhile, the cooling pipeline 8, the cooling liquid storage unit 9 and the cooling and power unit 10 dissipate heat for the semiconductor cooling fin group 3.
And step three, putting the solid slurry into a pre-freezing chamber, continuously freezing for at least 5 hours at the freezing temperature of minus 50 ℃, then carrying out freeze drying, and taking out after 24 hours of freeze drying to obtain the original embryo body.
And step four, sintering the original blank to obtain the porous framework, wherein the sintering time is 2-5h, and the sintering temperature is less than the melting point of the powder.
And step five, placing the melt-leaching material around the porous framework, immersing the porous framework, then heating and melt-leaching, wherein the heating temperature is higher than the melting point of the melt-leaching material and lower than the melting point of the framework powder, and cooling and solidifying at room temperature after the heating is finished to obtain the laminated composite material. The melt-leaching material is metal, macromolecule or mixed material of macromolecule and ceramic, and the melting point of the melt-leaching material is less than that of the powder.
Example 1
The embodiment provides a preparation method of a bionic oriented ordered laminated composite material, which comprises the following steps:
step one, preparing frozen casting slurry: the slurry comprises xanthan gum solution, polyvinyl alcohol and powder, and the powder comprises TiH2And B4C。
Specifically, 1.2g/L xanthan gum solution is prepared, and 40g of TiH with the diameter of 3 microns is added2Powder, 0.6gB4And C, uniformly mixing the powder C and 0.4g of polyvinyl alcohol, and adding the mixture into 92mL of xanthan gum solution, wherein the powder accounts for 10 percent of the total volume of the slurry. And stirring by adopting a high-energy ball mill, wherein the ball is a zirconia ball. Ball milling rotation speed is 200r/min, ball material ratio is 2:1, ball milling is carried out for 8 hours, and then the ball is taken out and bubble is removed.
And step two, directionally freezing the frozen casting slurry by adopting a freezing device shown in figure 1. And placing the mould on a copper sheet, slowly pouring the frozen casting slurry, adjusting the cooling rate to be 10 ℃/min and the cooling temperature to be-30 ℃, and freezing until the surface is completely frozen to obtain the solid slurry.
And step three, putting the frozen solid slurry into a pre-freezing chamber to continue freezing for 5 hours at the freezing temperature of-50 ℃, then carrying out freeze drying, and taking out after 24 hours of freeze drying to obtain the original embryo body.
Step four, the original blank is sent to vacuum sinteringSintering in a sintering furnace at 1300 deg.C and 10 deg.C- 3Pa, and the sintering time is 2h, thus obtaining the porous framework.
And step five, adopting high polymer resin as a melt-impregnation material. 100g of resin is placed around the porous framework, the porous framework is immersed, and the porous framework is placed into a vacuum sintering furnace to be heated until the resin is melted and immersed, wherein the heating temperature is 150 ℃. Taking out, cooling and solidifying at room temperature to obtain the resin-titanium laminated composite material. The structure of the optical microscope is shown in FIG. 2, from which the material stack can be seen.
Example 2
The embodiment provides a preparation method of a bionic oriented ordered laminated composite material, which comprises the following steps:
step one, preparing frozen casting slurry: the slurry comprises xanthan gum solution, polyvinyl alcohol and powder, and the powder comprises TiH2And B4C。
Specifically, 1.2g/L xanthan gum solution is prepared, and 40g of TiH with the diameter of 3 microns is added2Powder, 0.6gB4And C, uniformly mixing the powder C and 0.4g of polyvinyl alcohol, and adding the mixture into 64mL of xanthan gum solution, wherein the percentage of the powder in the total volume of the slurry is 20%. And stirring by adopting a high-energy ball mill, wherein the ball is a zirconia ball. Ball milling rotation speed is 200r/min, ball material ratio is 2:1, ball milling is carried out for 8 hours, and then the ball is taken out and bubble is removed.
And step two, directionally freezing the frozen casting slurry by adopting a freezing device shown in figure 1. And placing the mould on a copper sheet, slowly pouring the frozen casting slurry, adjusting the cooling rate to be 10 ℃/min and the cooling temperature to be-30 ℃, and freezing until the surface is completely frozen to obtain the solid slurry.
And step three, putting the frozen solid slurry into a pre-freezing chamber to continue freezing for 5 hours at the freezing temperature of-50 ℃, then carrying out freeze drying, and taking out after 24 hours of freeze drying to obtain the original embryo body.
Step four, the original blank is sent into a vacuum sintering furnace for sintering, the sintering temperature is 1300 ℃, and the vacuum degree is 10- 3Pa, and the sintering time is 2h, thus obtaining the porous framework.
And step five, adopting high polymer resin as a melt-impregnation material. 100g of resin is placed around the porous framework, the porous framework is immersed, and the porous framework is placed into a vacuum sintering furnace to be heated until the resin is melted and immersed, wherein the heating temperature is 150 ℃. Taking out, cooling and solidifying at room temperature to obtain the resin-titanium laminated composite material. The structure of the optical microscope is shown in FIG. 3, from which the material stack can be seen.
Example 3
The embodiment provides a preparation method of a bionic oriented ordered laminated composite material, which comprises the following steps:
step one, preparing frozen casting slurry: the slurry comprises xanthan gum solution, polyvinyl alcohol and powder, and the powder comprises TiH2And B4C。
Specifically, 1.2g/L xanthan gum solution is prepared, and 40g of TiH with the diameter of 3 microns is added2Powder, 0.6gB4And C, uniformly mixing the powder C and 0.4g of polyvinyl alcohol, and adding the mixture into 24mL of xanthan gum solution, wherein the powder accounts for 30 percent of the total volume of the slurry. And stirring by adopting a high-energy ball mill, wherein the ball is a zirconia ball. Ball milling rotation speed is 200r/min, ball material ratio is 2:1, ball milling is carried out for 8 hours, and then the ball is taken out and bubble is removed.
And step two, directionally freezing the frozen casting slurry by adopting a freezing device shown in figure 1. And placing the mould on a copper sheet, slowly pouring the frozen casting slurry, adjusting the cooling rate to be 10 ℃/min and the cooling temperature to be-30 ℃, and freezing until the surface is completely frozen to obtain the solid slurry.
And step three, putting the frozen solid slurry into a pre-freezing chamber to continue freezing for 5 hours at the freezing temperature of-50 ℃, then carrying out freeze drying, and taking out after 24 hours of freeze drying to obtain the original embryo body.
Step four, the original blank is sent into a vacuum sintering furnace for sintering, the sintering temperature is 1300 ℃, and the vacuum degree is 10- 3Pa, and the sintering time is 2h, thus obtaining the porous framework.
And step five, adopting high polymer resin as a melt-impregnation material. 100g of resin is placed around the porous framework, the porous framework is immersed, and the porous framework is placed into a vacuum sintering furnace to be heated until the resin is melted and immersed, wherein the heating temperature is 150 ℃. Taking out, cooling and solidifying at room temperature to obtain the resin-titanium laminated composite material. The structure of the optical microscope is shown in FIG. 4, from which the material stack can be seen.
Example 4
The embodiment provides a preparation method of a bionic oriented ordered laminated composite material, which comprises the following steps:
step one, preparing frozen casting slurry: the slurry comprises xanthan gum solution, polyvinyl alcohol and powder, and the powder comprises TiH2And B4C。
Specifically, 1.2g/L xanthan gum solution is prepared, and 40g of TiH with the diameter of 3 microns is added2Powder, 0.6gB4And C, uniformly mixing the powder C and 0.4g of polyvinyl alcohol, and adding the mixture into 24mL of xanthan gum solution, wherein the powder accounts for 30 percent of the total volume of the slurry. And stirring by adopting a high-energy ball mill, wherein the ball is a zirconia ball. Ball milling rotation speed is 200r/min, ball material ratio is 2:1, ball milling is carried out for 8 hours, and then the ball is taken out and bubble is removed.
And step two, directionally freezing the frozen casting slurry by adopting a freezing device shown in figure 1. And placing the mould on a copper sheet, slowly pouring the frozen casting slurry, adjusting the cooling rate to be 10 ℃/min and the cooling temperature to be-30 ℃, and freezing until the surface is completely frozen to obtain the solid slurry.
And step three, putting the frozen solid slurry into a pre-freezing chamber to continue freezing for 5 hours at the freezing temperature of-50 ℃, then carrying out freeze drying, and taking out after 24 hours of freeze drying to obtain the original embryo body.
Step four, the original blank is sent into a vacuum sintering furnace for sintering, the sintering temperature is 1300 ℃, and the vacuum degree is 10- 3Pa, and the sintering time is 2h, thus obtaining the porous framework.
Step five, adopting resin and TiB2The powder acts as a melt-leaching material. Heating and melting 100g of resin, and adding 1g of micron-sized TiB2The powders were blended. Pouring the mixture around the porous framework, immersing the porous framework, and putting the porous framework into a vacuum sintering furnace for melt-impregnation, wherein the heating temperature is 150 ℃. Taking out, cooling and solidifying at room temperature to obtain the resin doped TiB2-a titanium laminate composite. It is composed ofOptical microscopy structure the structure of the stack of materials is shown in figure 5, from which the structure can be seen.
Example 5
The embodiment provides a preparation method of a bionic oriented ordered laminated composite material, which comprises the following steps:
step one, preparing frozen casting slurry: the slurry comprises xanthan gum solution, polyvinyl alcohol and powder, and the powder comprises TiH2And B4C。
Specifically, 1.2g/L xanthan gum solution is prepared, and 40g of TiH with the diameter of 50 microns is added2Powder, 0.6gB4And C, uniformly mixing the powder C and 0.4g of polyvinyl alcohol, and adding the mixture into 64mL of xanthan gum solution, wherein the percentage of the powder in the total volume of the slurry is 20%. And stirring by adopting a high-energy ball mill, wherein the ball is a zirconia ball. Ball milling rotation speed is 200r/min, ball material ratio is 2:1, ball milling is carried out for 8 hours, and then the ball is taken out and bubble is removed.
And step two, directionally freezing the frozen casting slurry by adopting a freezing device shown in figure 1. And placing the mould on a copper sheet, slowly pouring the frozen casting slurry, adjusting the cooling rate to be 10 ℃/min and the cooling temperature to be-30 ℃, and freezing until the surface is completely frozen to obtain the solid slurry.
And step three, putting the frozen solid slurry into a pre-freezing chamber to continue freezing for 5 hours at the freezing temperature of-50 ℃, then carrying out freeze drying, and taking out after 24 hours of freeze drying to obtain the original embryo body.
Step four, the original blank is sent into a vacuum sintering furnace for sintering, the sintering temperature is 1300 ℃, and the vacuum degree is 10- 3Pa, and the sintering time is 2h, thus obtaining the porous framework.
And step five, adopting high polymer resin as a melt-impregnation material. 100g of resin is placed around the porous framework, the porous framework is immersed, and the porous framework is placed into a vacuum sintering furnace to be heated until the resin is melted and immersed, wherein the heating temperature is 150 ℃. Taking out, cooling and solidifying at room temperature to obtain the resin-titanium laminated composite material. The structure of the optical microscope is shown in FIG. 6, from which the material stack can be seen.
Example 6
The embodiment provides a preparation method of a bionic oriented ordered laminated composite material, which comprises the following steps:
step one, preparing frozen casting slurry: the slurry comprises xanthan gum solution, polyvinyl alcohol and powder, and the powder comprises TiH2And B4C。
Specifically, 1.2g/L xanthan gum solution is prepared, and 40g of TiH with the diameter of 100 microns is added2Powder, 0.6gB4And C, uniformly mixing the powder C and 0.4g of polyvinyl alcohol, and adding the mixture into 64mL of xanthan gum solution, wherein the percentage of the powder in the total volume of the slurry is 20%. And stirring by adopting a high-energy ball mill, wherein the ball is a zirconia ball. Ball milling rotation speed is 200r/min, ball material ratio is 2:1, ball milling is carried out for 8 hours, and then the ball is taken out and bubble is removed.
And step two, directionally freezing the frozen casting slurry by adopting a freezing device shown in figure 1. And placing the mould on a copper sheet, slowly pouring the frozen casting slurry, adjusting the cooling rate to be 10 ℃/min and the cooling temperature to be-30 ℃, and freezing until the surface is completely frozen to obtain the solid slurry.
And step three, putting the frozen solid slurry into a pre-freezing chamber to continue freezing for 5 hours at the freezing temperature of-50 ℃, then carrying out freeze drying, and taking out after 24 hours of freeze drying to obtain the original embryo body.
Step four, the original blank is sent into a vacuum sintering furnace for sintering, the sintering temperature is 1300 ℃, and the vacuum degree is 10- 3Pa, and the sintering time is 2h, thus obtaining the porous framework.
And step five, adopting high polymer resin as a melt-impregnation material. 100g of resin is placed around the porous framework, the porous framework is immersed, and the porous framework is placed into a vacuum sintering furnace to be heated until the resin is melted and immersed, wherein the heating temperature is 150 ℃. Taking out, cooling and solidifying at room temperature to obtain the resin-titanium laminated composite material. The structure of the optical microscope is shown in FIG. 7, from which the material stack can be seen.
Example 7
The embodiment provides a preparation method of a bionic oriented ordered laminated composite material, which comprises the following steps:
step one, preparing frozen casting slurry:the slurry comprises xanthan gum solution, polyvinyl alcohol and powder, and the powder comprises TiH2And B4C。
Specifically, 1.2g/L xanthan gum solution is prepared, and 40g of TiH with the diameter of 50 microns is added2Powder, 0.6gB4And C, uniformly mixing the powder C and 0.4g of polyvinyl alcohol, and adding the mixture into 64mL of xanthan gum solution, wherein the percentage of the powder in the total volume of the slurry is 20%. And stirring by adopting a high-energy ball mill, wherein the ball is a zirconia ball. Ball milling rotation speed is 200r/min, ball material ratio is 2:1, ball milling is carried out for 8 hours, and then the ball is taken out and bubble is removed.
And step two, directionally freezing the frozen casting slurry by adopting a freezing device shown in figure 1. And placing the mould on a copper sheet, slowly pouring the frozen casting slurry, adjusting the cooling rate to be 10 ℃/min and the cooling temperature to be-30 ℃, and freezing until the surface is completely frozen to obtain the solid slurry.
And step three, putting the frozen solid slurry into a pre-freezing chamber to continue freezing for 5 hours at the freezing temperature of-50 ℃, then carrying out freeze drying, and taking out after 24 hours of freeze drying to obtain the original embryo body.
Step four, the original blank is sent into a vacuum sintering furnace for sintering, the sintering temperature is 1300 ℃, and the vacuum degree is 10- 3Pa, and the sintering time is 2h, thus obtaining the porous framework.
And step five, adopting metal aluminum as a melting and leaching material. And putting the porous framework and the pure aluminum block into a crucible, immersing the porous framework in the pure aluminum, and feeding the porous framework into a vacuum sintering furnace to be heated until the aluminum block is molten, wherein the heating temperature is 700 ℃. And after the temperature is kept for ten minutes, cooling and solidifying the mixture along with the furnace to obtain the aluminum-titanium laminated composite material. The optical microscope structure and EDS diagram are shown in FIG. 8, from which the material stack structure can be seen.
Example 8
The embodiment provides a preparation method of a bionic oriented ordered laminated composite material, which comprises the following steps:
step one, preparing frozen casting slurry: the slurry comprises xanthan gum solution, polyvinyl alcohol and powder, and the powder comprises TiH2And B4C。
Specifically, 1.2g/L of xanthan gum is preparedSolution 40g of TiH with a diameter of 3 μm2Powder, 0.6gB4And C, uniformly mixing the powder C and 0.4g of polyvinyl alcohol, and adding the mixture into 24mL of xanthan gum solution, wherein the powder accounts for 30 percent of the total volume of the slurry. And stirring by adopting a high-energy ball mill, wherein the ball is a zirconia ball. Ball milling rotation speed is 200r/min, ball material ratio is 2:1, ball milling is carried out for 8 hours, and then the ball is taken out and bubble is removed.
And step two, directionally freezing the frozen casting slurry by adopting a freezing device shown in figure 1. And placing the mould on a copper sheet, slowly pouring the frozen casting slurry, adjusting the cooling rate to be 10 ℃/min and the cooling temperature to be-30 ℃, and freezing until the surface is completely frozen to obtain the solid slurry.
And step three, putting the frozen solid slurry into a pre-freezing chamber to continue freezing for 5 hours at the freezing temperature of-50 ℃, then carrying out freeze drying, and taking out after 24 hours of freeze drying to obtain the original embryo body.
Step four, the original blank is sent into a vacuum sintering furnace for sintering, the sintering temperature is 1300 ℃, and the vacuum degree is 10- 3Pa, and the sintering time is 2h, thus obtaining the porous framework.
And step five, adopting metal aluminum as a melting and leaching material. And putting the porous framework and the pure aluminum block into a crucible, immersing the porous framework in the pure aluminum, and feeding the porous framework into a vacuum sintering furnace to be heated until the aluminum block is molten, wherein the heating temperature is 700 ℃. And after the temperature is kept for ten minutes, cooling and solidifying the mixture along with the furnace to obtain the aluminum-titanium laminated composite material. The optical microscope structure and EDS diagram is shown in FIG. 9, from which the material stack structure can be seen.
Example 9
The embodiment provides a preparation method of a bionic oriented ordered laminated composite material, which comprises the following steps:
step one, preparing frozen casting slurry: the slurry comprises xanthan gum solution, polyvinyl alcohol and powder, and the powder comprises SiC and Ti.
Specifically, 1.2g/L xanthan gum solution is prepared, 40g of SiC powder with the diameter of 3 microns, 0.6g of Ti powder and 0.4g of polyvinyl alcohol are uniformly mixed and then added into 50mL of xanthan gum solution, namely the percentage of the powder in the total volume of the slurry is 25%. And stirring by adopting a high-energy ball mill, wherein the ball is a zirconia ball. Ball milling rotation speed is 200r/min, ball material ratio is 2:1, ball milling is carried out for 8 hours, and then the ball is taken out and bubble is removed.
And step two, directionally freezing the frozen casting slurry by adopting a freezing device shown in figure 1. And placing the mould on a copper sheet, slowly pouring the frozen casting slurry, adjusting the cooling rate to be 10 ℃/min and the cooling temperature to be-30 ℃, and freezing until the surface is completely frozen to obtain the solid slurry.
And step three, putting the frozen solid slurry into a pre-freezing chamber to continue freezing for 5 hours at the freezing temperature of-50 ℃, then carrying out freeze drying, and taking out after 24 hours of freeze drying to obtain the original embryo body.
Step four, the original blank is sent into a vacuum sintering furnace for sintering, the sintering temperature is 1300 ℃, and the vacuum degree is 10- 3Pa, and the sintering time is 2h, thus obtaining the porous framework.
And step five, adopting high polymer resin as a melt-impregnation material. 100g of resin was placed around the porous skeleton, the porous skeleton was immersed, and the resin was heated in a vacuum sintering furnace at 150 ℃. Taking out, and cooling and solidifying at room temperature. And obtaining the resin-SiC laminated composite material.
Example 10
The embodiment provides a preparation method of a bionic oriented ordered laminated composite material, which comprises the following steps:
step one, preparing frozen casting slurry: the slurry comprises xanthan gum solution, polyvinyl alcohol and powder, and the powder comprises metal Ti.
Specifically, 1.2g/L xanthan gum solution is prepared, 40g of Ti powder with the diameter of 3 microns and 0.4g of polyvinyl alcohol are uniformly mixed and then added into 27mL of xanthan gum solution, namely the percentage of the powder in the total volume of the slurry is 25%. And stirring by adopting a high-energy ball mill, wherein the ball is a zirconia ball. Ball milling rotation speed is 200r/min, ball material ratio is 2:1, ball milling is carried out for 8 hours, and then the ball is taken out and bubble is removed.
And step two, directionally freezing the frozen casting slurry by adopting a freezing device shown in figure 1. And placing the mould on a copper sheet, slowly pouring the frozen casting slurry, adjusting the cooling rate to be 10 ℃/min and the cooling temperature to be-30 ℃, and freezing until the surface is completely frozen to obtain the solid slurry.
And step three, putting the frozen solid slurry into a pre-freezing chamber to continue freezing for 5 hours at the freezing temperature of-50 ℃, then carrying out freeze drying, and taking out after 24 hours of freeze drying to obtain the original embryo body.
Step four, the original blank is sent into a vacuum sintering furnace for sintering, the sintering temperature is 1300 ℃, and the vacuum degree is 10- 3Pa, and the sintering time is 2h, thus obtaining the porous framework.
And step five, adopting high polymer resin as a melt-impregnation material. 100g of resin was placed around the porous skeleton, the porous skeleton was immersed, and the resin was heated in a vacuum sintering furnace at 150 ℃. Taking out, and cooling and solidifying at room temperature. And obtaining the resin-titanium laminated composite material.
In this embodiment, the powder may also be replaced with a metal compound TiH2Or ceramics B4C。

Claims (10)

1. A preparation method of a bionic oriented ordered laminated composite material is characterized by comprising the following steps:
the method comprises the following steps:
step one, preparing frozen casting slurry: the slurry comprises xanthan gum solution, polyvinyl alcohol and powder, wherein the polyvinyl alcohol accounts for 1% of the mass of the powder, and the powder accounts for 20-30% of the total volume of the slurry; the powder is one or a mixture of metal, metal compound and ceramic; uniformly mixing all the components, and removing bubbles to obtain frozen casting slurry;
step two, guiding the frozen casting slurry into a mold, and directionally freezing until the surface is completely frozen to obtain solid slurry;
step three, putting the solid slurry into a pre-freezing chamber to continue freezing for at least 5h, then carrying out freeze drying, and taking out after 24h of freeze drying to obtain an original embryo body;
sintering the original blank to obtain a porous framework, wherein the sintering time is 2-5h, and the sintering temperature is less than the melting point of the powder;
placing the melt-leaching material around the porous framework, heating for melt-leaching, wherein the heating temperature is higher than the melting point of the melt-leaching material and lower than the melting point of the framework powder, and cooling and solidifying at room temperature after the heating is finished to obtain the laminated composite material;
the melt-leaching material is metal, macromolecule or the mixed material of macromolecule and ceramic.
2. The method for preparing the biomimetic oriented ordered laminated composite material according to claim 1, wherein the method comprises the following steps:
and in the fifth step, the porous framework is immersed in the melt-leaching material.
3. The method for preparing the biomimetic oriented ordered laminated composite material according to claim 1, wherein the method comprises the following steps:
wherein the freezing temperature in the third step is-50 ℃.
4. The method for preparing the biomimetic oriented ordered laminated composite material according to claim 1, wherein the method comprises the following steps:
wherein the powder is TiH2And B4C。
5. The method for preparing the biomimetic oriented ordered laminated composite material according to claim 1, wherein the method comprises the following steps:
wherein the melt-impregnated material is a resin.
6. The method for preparing the biomimetic oriented ordered laminated composite material according to claim 1, wherein the method comprises the following steps:
wherein the melt-leaching material is resin and TiB2。
7. The method for preparing the biomimetic oriented ordered laminated composite material according to claim 1, wherein the method comprises the following steps:
and in the fifth step, heating and melting and soaking by adopting a vacuum sintering furnace.
8. The method for preparing the biomimetic oriented ordered laminated composite material according to claim 1, wherein the method comprises the following steps:
the second step adopts a refrigerating device for directional refrigeration, wherein the refrigerating device comprises a mold, a metal sheet, a semiconductor refrigerating sheet group, a thermosensitive semiconductor, a temperature controller, a power supply, a metal hollow plate, a cooling pipeline, a cooling liquid storage unit and a cooling and power unit;
the mold is a frame body with a circle of closed side walls, and the material of the mold is heat-insulating material;
the die is arranged on the metal sheet, and the metal sheet is fixed on the semiconductor refrigerating sheet set;
the semiconductor refrigerating sheet set is connected with a power supply, the power supply supplies power to the semiconductor refrigerating sheet set, and the semiconductor refrigerating sheet set is electrified for refrigeration;
the temperature controller is connected with the thermosensitive semiconductor and monitors the temperature at the bottom of the die;
the temperature controller is also connected with a power supply and controls the refrigerating temperature and the cooling rate of the semiconductor refrigerating sheet set by adjusting the output of the power supply;
the semiconductor refrigerating sheet group is fixed on the metal hollow plate;
the cooling liquid storage unit is used for storing cooling liquid and is communicated with the metal hollow plate through a cooling pipeline to form a cooling loop so as to provide circulating cooling liquid for the metal hollow plate;
the cooling and power unit comprises a cooling device and a power device, is arranged on the cooling pipeline, and cools and conveys the cooling liquid.
9. The method for preparing the biomimetic oriented ordered laminated composite material according to claim 1, wherein the method comprises the following steps:
wherein, in the step one, the concentration of the xanthan gum solution is 1.2 g/L.
10. The method for preparing the biomimetic oriented ordered laminated composite material according to claim 1, wherein the method comprises the following steps:
in the first step, ball milling is adopted to mix the freezing casting slurry.
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