CN115448723A - Preparation method and application of boron carbide-based ceramic modified by magnesium-aluminum hydrotalcite - Google Patents
Preparation method and application of boron carbide-based ceramic modified by magnesium-aluminum hydrotalcite Download PDFInfo
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- CN115448723A CN115448723A CN202210809026.5A CN202210809026A CN115448723A CN 115448723 A CN115448723 A CN 115448723A CN 202210809026 A CN202210809026 A CN 202210809026A CN 115448723 A CN115448723 A CN 115448723A
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- boron carbide
- magnesium
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- aluminum hydrotalcite
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- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 53
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 53
- 229910052580 B4C Inorganic materials 0.000 title claims abstract description 48
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000000919 ceramic Substances 0.000 title claims abstract description 30
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 title claims abstract description 28
- HNDVDQJCIGZPNO-YFKPBYRVSA-N L-histidine Chemical compound OC(=O)[C@@H](N)CC1=CN=CN1 HNDVDQJCIGZPNO-YFKPBYRVSA-N 0.000 claims abstract description 46
- 239000000243 solution Substances 0.000 claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 26
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 229960002885 histidine Drugs 0.000 claims abstract description 23
- -1 magnesium-aluminum hydrotalcite modified boron carbide Chemical class 0.000 claims abstract description 23
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 17
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 238000002425 crystallisation Methods 0.000 claims abstract description 16
- 230000008025 crystallization Effects 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 15
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 238000009830 intercalation Methods 0.000 claims abstract description 9
- 230000002687 intercalation Effects 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000011261 inert gas Substances 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000002131 composite material Substances 0.000 claims description 16
- 229910044991 metal oxide Inorganic materials 0.000 claims description 15
- 150000004706 metal oxides Chemical class 0.000 claims description 15
- 239000000725 suspension Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 229910001051 Magnalium Inorganic materials 0.000 claims description 7
- 238000007598 dipping method Methods 0.000 claims description 5
- HHCCNQLNWSZWDH-UHFFFAOYSA-N n-hydroxymethanimine oxide Chemical compound O[N+]([O-])=C HHCCNQLNWSZWDH-UHFFFAOYSA-N 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 claims description 2
- 239000003575 carbonaceous material Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 238000004523 catalytic cracking Methods 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000002071 nanotube Substances 0.000 claims 1
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 238000000280 densification Methods 0.000 abstract description 5
- 238000005119 centrifugation Methods 0.000 abstract description 4
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract 1
- 238000005470 impregnation Methods 0.000 abstract 1
- 229910017604 nitric acid Inorganic materials 0.000 abstract 1
- 239000000463 material Substances 0.000 description 13
- 239000013078 crystal Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 238000009792 diffusion process Methods 0.000 description 6
- 239000011229 interlayer Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000005349 anion exchange Methods 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
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Abstract
The invention provides a preparation method of boron carbide modified by magnesium-aluminum hydrotalcite, which comprises the following steps: mixing magnesium nitrate and aluminum nitrate to obtain a nitrate aqueous solution; titrating a sodium hydroxide solution into an L-histidine solution to obtain an L-histidine base solution; placing the carbon nano tube purified by acid in a nitrogen environment, stirring vigorously, simultaneously adding aqueous solution of nitric acid and L-histidine base solution dropwise, stirring at constant temperature to perform intercalation impregnation reaction, performing crystallization treatment after the reaction is finished, performing centrifugation, washing, drying and calcination treatment in sequence after the crystallization treatment is finished, uniformly mixing the carbon nano tube with boron carbide micropowder, performing ball milling, tabletting and vacuum heating treatment in sequence, introducing inert gas, and cooling to room temperature to obtain magnesium-aluminum hydrotalcite modified boron carbide; through the technical scheme, the problem that the boron carbide ceramic material with strong high temperature and high pressure resistance and corrosion resistance is obtained due to the lack of the ability of effectively modifying the toughening and densification degree of the boron carbide ceramic in the prior art is solved.
Description
Technical Field
The invention relates to the field of composite materials, in particular to a preparation method and application of boron carbide-based ceramics modified by magnesium-aluminum hydrotalcite.
Background
Boron carbide-based ceramics are a novel material, have excellent properties of low specific gravity, high hardness and high strength, and are therefore widely used in the fields of personal protective equipment, protection of land vehicles, airplanes and helicopters, protection of small-caliber cannonballs, and the like. However, boron carbide, which is a compound having strong covalent bonds, has a much slower diffusion process in its crystal than that of an oxide, and thus suffers from the limitations of powder agglomeration and difficulty in forming a dense material having high mechanical properties in use, and further requires an extremely high temperature or application of external pressure.
In conclusion, the prior art lacks a method for effectively modifying the toughening and densification degree of boron carbide ceramic and obtaining the boron carbide ceramic material with simple preparation, strong high temperature and high pressure resistance and corrosion resistance.
Disclosure of Invention
In view of the above disadvantages of the prior art, the present invention aims to provide a method for preparing boron carbide-based ceramic modified with magnesium aluminum hydrotalcite, which is used to solve the problem that the prior art lacks a method capable of effectively modifying the toughening and densification degree of boron carbide ceramic and obtaining boron carbide ceramic material with simple preparation, strong high temperature and high pressure resistance and corrosion resistance.
In order to attain the above and other related objects,
the invention provides a preparation method of boron carbide modified by magnesium-aluminum hydrotalcite, which comprises the following steps:
s1, mixing magnesium nitrate and aluminum nitrate to obtain a nitrate aqueous solution;
s2, titrating the sodium hydroxide solution into an L-histidine solution until the pH value is 8.9-10.2 to obtain an L-histidine base solution;
s3, placing the carbon nano tube purified by acid in a nitrogen environment, violently stirring at the temperature of 20-40 ℃, simultaneously dropwise adding a nitronic acid aqueous solution and an L-histidine base solution, stirring at constant temperature to perform intercalation dipping reaction, and obtaining a suspension after the reaction is finished;
s4, crystallizing the suspension, and sequentially centrifuging, washing, drying and calcining after crystallization to obtain the magnalium hydrotalcite modified carbon nanotube composite metal oxide;
s5, uniformly mixing the carbon nanotube composite metal oxide modified by the magnesium-aluminum hydrotalcite and the boron carbide micro powder, sequentially performing ball milling, tabletting and vacuum heating treatment, introducing inert gas, and cooling to room temperature to obtain the magnesium-aluminum hydrotalcite modified boron carbide.
According to the technical scheme, the magnesium-aluminum hydrotalcite modified carbon nanotube material with the nitrate radical intercalation is used for modifying the toughening and compactness performance of boron carbide, L-histidine is used as a green and nontoxic chemical raw material, is decomposed to generate nitrate radicals under the conditions of high temperature and high pressure, is intercalated between magnesium-aluminum hydrotalcite laminates with carbon nanotubes, ensures the stable forming process of crystals through the hydrothermal process, and is roasted to obtain the carbon nanotube composite metal oxide with the laminate structure, so that the effective dispersion structure of the carbon nanotubes is improved fundamentally, and the crystal diffusion in the boron carbide body is facilitated.
In an embodiment of the invention, the concentration of magnesium nitrate in the nitrate aqueous solution in the step S1 is 1 to 2.5mol/L, and the concentration of aluminum nitrate is 0.5 to 0.8mol/L.
In an embodiment of the present invention, the concentration of the sodium hydroxide solution in step S2 is 1-1.5 mol/L, L-histidine solution is 0.25-0.5 mol/L.
In an embodiment of the invention, the solid-to-liquid ratio of the suspension in the step S3 is 1g:40 to 70ml.
In an embodiment of the present invention, in the step S3, the carbon nanotubes are in a fluidized bed reactor at a temperature of 700 ℃ and Fe-Ni/Al 2 O 3 Under the catalytic condition of a catalyst, a multi-wall carbon material synthesized by catalytic cracking of methane is boiled and washed by HClWashing and drying to obtain the multi-wall carbon nano tube.
In an embodiment of the present invention, the crystallization temperature in the step S4 is 120-200 ℃, and the crystallization time is 18-24 hours; the drying temperature is 80-150 ℃, and the drying time is 5-8 h; the calcining temperature is 500-750 ℃, and the calcining time is 5-7 h.
In an embodiment of the present invention, the crystallization in the step S4 is performed in a hydrothermal synthesis kettle.
In an embodiment of the present invention, in the step S5, the mass ratio of the magnesium aluminum hydrotalcite modified carbon nanotube composite metal oxide to the boron carbide fine powder is 0.08 to 0.5:1.
in an embodiment of the present invention, in the step S5, the ball milling rotation speed is 120 to 350r/min, and the ball milling time is 1 to 2 hours; the vacuum heating temperature is 1500-2200 ℃, the heating rate is 2-7 ℃/min per minute, and the heating time is 3-6 h.
The invention provides an application of magnesium-aluminum hydrotalcite modified boron carbide, in particular an application in the aspect of protecting small-caliber shells.
As described above, the preparation method and the application of the boron carbide modified by the magnesium-aluminum hydrotalcite of the invention have the following beneficial effects:
1. the added carbon nano tube is introduced in the preparation of the ceramic matrix, so that the fracture toughness can be obviously improved through toughening mechanisms such as fiber extraction, crack bridging, crack deflection and the like, and the carbon nano tube is obviously superior to other fiber materials in the aspects of structure or mechanics; the magnalium hydrotalcite has good anion exchange capacity, strong thermal stability and controllable interlayer spacing, can provide strong corrosion resistance and self-repairing capacity as a nano container, and is greatly beneficial to effective diffusion of a load carrier.
2. The magnesium-aluminum hydrotalcite modified carbon nanotube material with the nitrate radical intercalation is used for modifying the toughening and compactness performance of boron carbide, L-histidine is decomposed to generate nitrate radicals under the conditions of high temperature and high pressure, the nitrate radicals are intercalated between magnesium-aluminum hydrotalcite stratums with carbon nanotubes, the interlayer spacing of the structure of the magnesium-aluminum hydrotalcite stratums is effectively increased, the stable forming process of crystals is ensured through the hydrothermal process, and then the carbon nanotube composite metal oxide (MgAl-LDO @ CNT) with the interlayer structure is obtained through roasting. The effective dispersion structure of the carbon nano tube is improved fundamentally, the crystal diffusion in the boron carbide body is accelerated, the sintering temperature of the boron carbide material is effectively reduced, the densification degree of the material is improved, and the bending strength is improved.
Drawings
Fig. 1 is a schematic diagram showing the principle flow of steps S3 and S4 in boron carbide modified by magnesium-aluminum hydrotalcite in the embodiment of the present invention.
Fig. 2 is a schematic view showing a micro flow of steps S3 and S4 in boron carbide modified by magnesium aluminum hydrotalcite according to an embodiment of the present invention.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
The magnesium aluminum hydrotalcite modified boron carbide-based ceramics prepared in the following examples 1 to 3 can be used for preparing small-caliber protective cannonballs.
Example 1
A preparation method of boron carbide-based ceramic modified by magnesium-aluminum hydrotalcite comprises the following steps:
s1, mixing magnesium nitrate and aluminum nitrate to obtain 100ml of nitrate aqueous solution, wherein the concentration of the aluminum nitrate in the nitrate aqueous solution is 0.5mol/L, and the concentration of the magnesium nitrate is 1mol/L;
s2, titrating a sodium hydroxide solution with the concentration of 1mol/L into an L-histidine solution with the concentration of 0.3mol/L until the pH value is 8.9-9.2 to obtain an L-histidine base solution;
s3, weighing 2g of acid-purified carbon nano tube, placing the acid-purified carbon nano tube in a nitrogen environment, violently stirring at the temperature of 35 ℃, simultaneously dropwise adding a nitronic acid aqueous solution and an L-histidine base solution, stirring at constant temperature to perform intercalation dipping reaction, and obtaining a suspension after the reaction is finished;
s4, carrying out crystallization treatment on the suspension textile fabric in a hydrothermal synthesis kettle at the temperature of 160 ℃ for 20 hours, sequentially carrying out centrifugation and washing after the crystallization treatment is finished, drying at the temperature of 120 ℃ for 8 hours, and then carrying out calcination treatment at the temperature of 600 ℃ for 5 hours to obtain a magnesium-aluminum hydrotalcite modified carbon nanotube composite metal oxide (MgAl-LDO @ CNT);
s5, mixing the magnalium hydrotalcite modified carbon nano tube composite metal oxide and boron carbide micro powder in a proportion of 1: uniformly mixing the materials according to a mass ratio of 0.2, ball-milling for 2 hours at 300r/min, tabletting, heating in vacuum at 1600 ℃ for 3 hours, introducing inert gas, and cooling to room temperature to obtain the magnesium-aluminum hydrotalcite modified boron carbide-based ceramic.
Example 2
A preparation method of magnesium-aluminum hydrotalcite modified boron carbide-based ceramic comprises the following steps:
s1, mixing magnesium nitrate and aluminum nitrate to obtain 120ml of nitrate aqueous solution, wherein the concentration of the aluminum nitrate in the nitrate aqueous solution is 0.5mol/L, and the concentration of the magnesium nitrate is 1mol/L;
s2, titrating a sodium hydroxide solution with the concentration of 1mol/L into an L-histidine solution with the concentration of 0.3mol/L until the pH value is 8.9-9.2 to obtain an L-histidine base solution;
s3, weighing 3g of carbon nano tube subjected to acid purification, placing the carbon nano tube subjected to acid purification in a nitrogen environment, violently stirring at the temperature of 35 ℃, simultaneously dropwise adding a nitronic acid aqueous solution and an L-histidine base solution, stirring at constant temperature to perform intercalation dipping reaction, and obtaining a suspension after the reaction is finished;
s4, carrying out crystallization treatment on the suspension textile fabric in a hydrothermal synthesis kettle at the temperature of 200 ℃ for 18h, sequentially carrying out centrifugation and washing after the crystallization treatment is finished, drying at the temperature of 120 ℃ for 8h, and then carrying out calcination treatment at the temperature of 600 ℃ for 5h to obtain a magnesium-aluminum hydrotalcite modified carbon nanotube composite metal oxide (MgAl-LDO @ CNT);
s5, mixing the magnalium hydrotalcite modified carbon nanotube composite metal oxide and boron carbide micro powder in a proportion of 1: uniformly mixing the materials according to a mass ratio of 0.3, ball-milling for 2 hours at a speed of 250r/min, tabletting, heating in vacuum at 1600 ℃ for 3 hours, introducing inert gas, and cooling to room temperature to obtain the magnesium-aluminum hydrotalcite modified boron carbide-based ceramic.
Example 3
A preparation method of boron carbide-based ceramic modified by magnesium-aluminum hydrotalcite comprises the following steps:
s1, mixing magnesium nitrate and aluminum nitrate to obtain 160ml of nitrate aqueous solution, wherein the concentration of the aluminum nitrate in the nitrate aqueous solution is 0.5mol/L, and the concentration of the magnesium nitrate is 1mol/L;
s2, titrating a sodium hydroxide solution with the concentration of 1mol/L into an L-histidine solution with the concentration of 0.3mol/L until the pH value is 8.9-9.2 to obtain an L-histidine base solution;
s3, weighing 4g of acid-purified carbon nano tube, placing the acid-purified carbon nano tube in a nitrogen environment, violently stirring at the temperature of 35 ℃, simultaneously dropwise adding a nitronic acid aqueous solution and an L-histidine base solution, stirring at constant temperature to perform intercalation dipping reaction, and obtaining a suspension after the reaction is finished;
s4, carrying out crystallization treatment on the suspension textile fabric in a hydrothermal synthesis kettle at 220 ℃ for 22h, sequentially carrying out centrifugation and washing after the crystallization treatment is finished, drying at 120 ℃ for 8h, and then calcining at 600 ℃ for 5h to obtain a magnesium-aluminum hydrotalcite modified carbon nanotube composite metal oxide (MgAl-LDO @ CNT);
s5, mixing the magnalium hydrotalcite modified carbon nano tube composite metal oxide and boron carbide micro powder in a proportion of 1: uniformly mixing the raw materials according to the mass ratio of 0.5, ball-milling for 2h at 350r/min, tabletting, heating at 1600 ℃ in vacuum for 4h, introducing inert gas, and cooling to room temperature to obtain the boron carbide-based ceramic modified by the magnesium-aluminum hydrotalcite.
Comparative example 1
Ball-milling boron carbide micro powder for 2h at the speed of 300r/min, tabletting, heating in vacuum at 1600 ℃ for 3h, introducing inert gas, and cooling to room temperature to obtain the boron carbide-based ceramic.
Performance testing
The process parameters in examples 1-3 and comparative example 1 are shown in table 1.
TABLE 1
The performance characteristics of the materials of examples 1-3 and comparative example 1 are shown in table 2.
TABLE 2
Density of material (g/cm) 3 ) | Flexural Strength (MPa) | |
Example 1 | 2.97 | 480 |
Example 2 | 3.15 | 497 |
Example 3 | 2.86 | 467 |
Comparative example 1 | 2.37 | 350 |
As can be seen from tables 1 and 2,
comparative example 1 does not introduce modification with magnesium aluminum hydrotalcite, and the boron carbide-based ceramic obtained by directly using boron carbide micropowder as a main raw material has a material density lower than that of the boron carbide-based ceramic modified with magnesium aluminum hydrotalcite prepared in examples 1 to 3, and has a lower material density and a lower bending strength, because the magnesium aluminum hydrotalcite modified carbon nanotube material with nitrate intercalation acts on modification of toughening and densification properties of boron carbide, L-histidine is decomposed at high temperature and high pressure to generate nitrate, and the nitrate is intercalated between magnesium aluminum hydrotalcite layers with carbon nanotubes, so that the interlayer spacing of the structure is effectively increased, the stable forming process of the crystal is ensured through the hydrothermal process, and then the carbon nanotube composite metal oxide (MgAl-ldo @ cnt) with the interlayer structure is obtained by roasting. The effective dispersion structure of the carbon nano tube is improved fundamentally, and the crystal diffusion in the boron carbide body is accelerated.
In conclusion, the addition of the carbon nanotubes in the preparation of the ceramic matrix can obviously improve fracture toughness through toughening mechanisms such as fiber extraction, crack bridging, crack deflection and the like, and is obviously superior to other fiber materials in structural or mechanical aspects; the magnalium hydrotalcite has good anion exchange capacity, strong thermal stability and controllable interlayer spacing, can provide strong corrosion resistance and self-repairing capacity as a nano container, and is greatly beneficial to effective diffusion of a load carrier. Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A preparation method of magnesium-aluminum hydrotalcite modified boron carbide-based ceramic is characterized by comprising the following steps:
s1, mixing magnesium nitrate and aluminum nitrate to obtain a nitrate aqueous solution;
s2, titrating the sodium hydroxide solution into an L-histidine solution until the pH value is 8.9-10.2 to obtain an L-histidine base solution;
s3, placing the carbon nano tube purified by acid in a nitrogen environment, violently stirring at the temperature of 20-40 ℃, simultaneously dropwise adding a nitronic acid aqueous solution and an L-histidine base solution, stirring at constant temperature to perform intercalation dipping reaction, and obtaining a suspension after the reaction is finished;
s4, crystallizing the suspension, and sequentially centrifuging, washing, drying and calcining after crystallization to obtain the magnalium hydrotalcite modified carbon nanotube composite metal oxide;
and S5, uniformly mixing the carbon nanotube composite metal oxide modified by the magnesium-aluminum hydrotalcite with the boron carbide micro powder, sequentially performing ball milling, tabletting and vacuum heating treatment, introducing inert gas, and cooling to room temperature to obtain the magnesium-aluminum hydrotalcite modified boron carbide.
2. The preparation method of the boron carbide-based ceramic modified by the magnesium aluminum hydrotalcite of claim 1, wherein the preparation method comprises the following steps: the concentration of magnesium nitrate in the nitrate aqueous solution in the step S1 is 1-2.5 mol/L, and the concentration of aluminum nitrate is 0.5-0.8 mol/L.
3. The preparation method of the boron carbide-based ceramic modified by the magnesium aluminum hydrotalcite of claim 1, wherein the preparation method comprises the following steps: the concentration of the sodium hydroxide solution in the step S2 is 1-1.5 mol/L, L-histidine solution is 0.25-0.5 mol/L.
4. The preparation method of the boron carbide-based ceramic modified by the magnesium-aluminum hydrotalcite according to claim 1, wherein the preparation method comprises the following steps: the solid-to-liquid ratio of the suspension in the step S3 is 1g:40 to 70ml.
5. The preparation method of the boron carbide-based ceramic modified by the magnesium aluminum hydrotalcite of claim 1, wherein the preparation method comprises the following steps: in the step S3, the carbon nano tube is in a fluidized bed reactor at the temperature of 700 ℃ and Fe-Ni/Al 2 O 3 Under the catalytic condition of a catalyst, a multi-wall carbon material is synthesized by catalytic cracking of methane, boiled, washed and dried by HCl to obtain the multi-wall carbon materialCarbon nanotubes.
6. The preparation method of the boron carbide-based ceramic modified by the magnesium aluminum hydrotalcite of claim 1, wherein the preparation method comprises the following steps: in the step S4, the crystallization temperature is 120-200 ℃, and the crystallization time is 18-24 h; the drying temperature is 80-150 ℃, and the drying time is 5-8 h; the calcining temperature is 500-750 ℃, and the calcining time is 5-7 h.
7. The preparation method of the boron carbide-based ceramic modified by the magnesium aluminum hydrotalcite of claim 1, wherein the preparation method comprises the following steps: and the crystallization in the step S4 is carried out in a hydrothermal synthesis kettle.
8. The preparation method of the boron carbide-based ceramic modified by the magnesium aluminum hydrotalcite of claim 1, wherein the preparation method comprises the following steps: in the step S5, the mass ratio of the magnesium-aluminum hydrotalcite modified carbon nano tube composite metal oxide to the boron carbide micro powder is 0.08-0.5: 1.
9. the preparation method of the boron carbide-based ceramic modified by the magnesium aluminum hydrotalcite of claim 1, wherein the preparation method comprises the following steps: in the step S5, the ball milling speed is 120-350 r/min, and the ball milling time is 1-2h; the vacuum heating temperature is 1500-2200 ℃, the heating rate is 2-7 ℃/min per minute, and the heating time is 3-6 h.
10. Use of the magnesium aluminum hydrotalcite modified boron carbide-based ceramic according to any of claims 1 to 9,
the application in the aspect of protecting small-caliber shells.
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