CN113336553A - V2AlC bulk material synthesized by microwave sintering and preparation method and application thereof - Google Patents
V2AlC bulk material synthesized by microwave sintering and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a microwave sintering synthetic V2The AlC bulk material and the preparation method thereof comprise the following steps: according to V: al: c =2 (1.1-1.4) and 1, vanadium powder, aluminum powder and graphite powder are weighed according to the molar ratio of 1, and sintering aid LaF is added3Or CeF3Adding the powder into absolute ethyl alcohol, grinding for 30min by using a quartz mortar, and drying for 5h in vacuum at 50 ℃ to obtain a mixed raw material; placing the mixed raw materials in a steel grinding tool, and pressing for 60s under the pressure of 240MPa to form a cylindrical blank; placing the pressed blank in a microwave sintering device, heating to 1250 ℃ in argon atmosphere, preserving heat for 5min, and cooling to obtain V2Bulk material of AlC.
Description
Technical Field
The invention relates to the field of inorganic non-metallic materials, in particular to a microwave sintering synthetic V2AlC bulk material and a preparation method and application thereof.
Background
V2AlC is a ternary transition metal carbide, belonging to one of the MAX phases, which combines the excellent properties of ceramics and metals, such as a lower density (4.07 g/cm)３) High modulus (283 GPa) and good conductivity (4 multiplied by 10)6S·m-1) And thermal conductivity (48 W.m)-1·K-1) Excellent oxidation resistance (below 500 ℃), thermal shock resistance, good high pressure resistance and excellent processing performance. Thus, V2The AlC material can be used as wear-resistant material, reinforcing phase material of metal matrix composite material, heating element, nozzle and the like.
Synthesis of V2The AlC method comprises hot isostatic pressing, hot pressing, spark plasma sintering and the like, and the hot isostatic pressing method is adopted to prepare compact V by a 1600 ℃/8 h process2An AlC polycrystalline material; in-situ hot pressing sintering process of preparing compact single-phase V2AlC polycrystalline material is generally carried out at 1400-1600 ℃ under the condition of heat preservation for 1 h. These processes are mainly used for the preparation of bulk V2The defects of overhigh synthesis temperature, long sintering time and low purity of AlC generally exist.
Disclosure of Invention
The invention aims to solve the problem of the prior V2The problems of high temperature, long synthesis time and low purity in the synthesis of AlC block materials are solved, and the method for synthesizing high-purity V at lower temperature in short time is provided2Method for preparing AlC bulk material and V prepared by method2Application of AlC block material in wear-resistant material and V2And C, application of a precursor material of the two-dimensional material.
Based on the purpose, the invention adopts the following technical scheme:
microwave sintering synthesis of V2A method of forming a bulk material of AlC comprising the steps of:
a. adding vanadium powder, aluminum powder, graphite powder and sintering aid into absolute ethyl alcohol, grinding, uniformly mixing, and vacuum drying to obtain a mixed raw material; the sintering aid is rare earth fluoride;
b. pressing the mixed raw materials into a blank in a mould;
c. placing the embryo body in a micro-chamberHeating in vacuum or inert atmosphere in a wave sintering device, and cooling to room temperature to obtain V2Bulk material of AlC.
Further, the sintering aid is LaF3Or CeF3。
Further, the molar ratio of the vanadium powder to the aluminum powder to the graphite powder is V to Al to C =2 (1.1-1.4) to 1, and the sintering aid accounts for 2% -4% of the sum of the mass of the vanadium powder, the mass of the aluminum powder and the mass of the graphite powder.
Further, the reaction conditions of the microwave sintering are that the frequency of the microwave sintering is 2.45GHz, the power is 900W, the heating rate of the microwave heating in the step c is 100 ℃/min, the temperature is kept for 5min when the temperature is raised to 1250 ℃, and the inert atmosphere is argon.
Further, in the step a, the mixing manner is ground for 30min by using a quartz mortar, and the vacuum drying temperature is 50 ℃.
Further, the pressure of the die pressing in the step b is 240MPa, and the pressing time is 60 s.
V prepared by the above method2The AlC bulk material has fine grains and uniform microstructure.
V prepared by the method2AlC bulk materials, because of their high purity and high density, are widely used in wear resistant materials and V2C precursor material of two-dimensional material.
The invention has the beneficial effects that:
(1) the invention fully utilizes the heating characteristic of microwave sintering, utilizes the high-efficiency internal heating mode of microwave and the direct supply and permeation of energy in the synthesis process of uniformly mixed raw materials, strengthens the diffusion process of energy, avoids the problem of nonuniform microstructure and ensures that the synthesized V has uniform structure2The crystal grains of the AlC bulk material are fine, and the microstructure is uniform.
(2) The invention adopts a microwave sintering heating mode, and directly adopts V during material preparation2The atomic ratio of AlC, the addition of the raw materials are controlled, other impurities are prevented from being introduced, the heating rate in the microwave heating process is high, the heating rate can reach 100 ℃/min, and V is obtained after the sintering aid is added2Greatly shortens the AlC synthesis time and can effectively inhibit aluminum powderThe energy consumption is greatly reduced, and the production efficiency is improved.
(3) In the course of the reaction, LaF3Or CeF3The addition of the sintering aid increases the liquid phase amount of the material in the microwave heating process, is favorable for element diffusion and is favorable for synthesizing V2AlC reaction, and synthesized V2The purity of AlC is improved.
Drawings
FIG. 1 Synthesis of V in example 12The X-ray diffraction spectrum of AlC;
FIG. 2 shows the synthesis V of comparative example 2, comparative example 3, example 1 and example 3 in comparison2The X-ray diffraction spectrum of AlC;
FIG. 3 Synthesis of V in example 12Scanning electron micrograph of AlC.
Detailed Description
Comparative example 1
Pressureless sintering synthesis of V2A method of forming a bulk material of AlC comprising the steps of:
a. weighing 2.09g of vanadium powder, 0.66g of aluminum powder and 0.25g of graphite powder according to the molar ratio of V to Al to C =2 to 1.2 to 1, adding the powder into 5ml of absolute ethyl alcohol, grinding for 30min by using a quartz mortar, and drying for 5h in vacuum at 50 ℃ to obtain a mixed raw material;
b. and pressing the mixed raw materials in a hydraulic press for 60s under the pressure of 10MPa to form a cylindrical blank.
c. Placing the pressed blank in a tube furnace, heating to 1250 ℃ in argon atmosphere, preserving heat for 90min, and cooling to obtain V2Bulk material of AlC.
Comparative example 2
Pressureless sintering synthesis of V2A method of forming a bulk material of AlC comprising the steps of:
a. weighing 2.09g of vanadium powder, 0.66g of aluminum powder and 0.25g of graphite powder according to the molar ratio of V to Al to C =2 to 1.2 to 1, and adding 0.06g of LaF3(2%) as a sintering aid, adding the powder into 5ml of absolute ethyl alcohol, grinding for 30min by using a quartz mortar, and drying in vacuum at 50 ℃ for 5h to obtain a mixed raw material;
b. and (3) pressing the mixed raw materials in a steel grinding tool for 60s under the pressure of 240MPa to form a cylindrical blank.
c. Placing the pressed blank in a tube furnace, heating to 1250 ℃ in argon atmosphere, preserving heat for 90min, and cooling to obtain V2Bulk material of AlC.
Comparative example 3
Microwave sintering synthesis of V2A method of forming a bulk material of AlC comprising the steps of:
a. weighing 2.09g of vanadium powder, 0.66g of aluminum powder and 0.25g of graphite powder according to the molar ratio of V to Al to C =2 to 1.2 to 1, adding the powder into 5ml of absolute ethyl alcohol without adding a sintering aid, grinding for 30min by using a quartz mortar, and drying for 5h in vacuum at 50 ℃ to obtain a mixed raw material;
b. and (3) pressing the mixed raw materials in a steel grinding tool for 60s under the pressure of 240MPa to form a cylindrical blank.
c. Placing the pressed blank in a microwave sintering device, heating to 1250 ℃ in argon atmosphere, preserving heat for 5min, and cooling to obtain V2Bulk material of AlC.
Example 1
Microwave sintering synthesis of V2A method of forming a bulk material of AlC comprising the steps of:
a. weighing 2.09g of vanadium powder, 0.66g of aluminum powder and 0.25g of graphite powder according to the molar ratio of V to Al to C =2 to 1.2 to 1, and adding 0.12g of LaF3(4%) as a sintering aid, adding the powder into 5ml of absolute ethyl alcohol, grinding for 30min by using a quartz mortar, and drying in vacuum at 50 ℃ for 5h to obtain a mixed raw material;
b. and (3) pressing the mixed raw materials in a steel grinding tool for 60s under the pressure of 240MPa to form a cylindrical blank.
c. Placing the pressed blank in a microwave sintering device, heating to 1250 ℃ in argon atmosphere, preserving heat for 5min, and cooling to obtain V2Bulk material of AlC.
Example 2
Microwave sintering synthesis of V2A method of forming a bulk material of AlC comprising the steps of:
a. weighing 2.09g of vanadium powder, 0.66g of aluminum powder and 0.25g of graphite powder according to the molar ratio of V to Al to C =2 to 1.2 to 1, and adding 0.06g of LaF3(2%) as a sintering aid,adding the powder into 5ml of absolute ethyl alcohol, grinding for 30min by using a quartz mortar, and drying for 5h in vacuum at 50 ℃ to obtain a mixed raw material;
b. and (3) pressing the mixed raw materials in a steel grinding tool for 60s under the pressure of 240MPa to form a cylindrical blank.
c. Placing the pressed blank in a microwave sintering device, heating to 1250 ℃ in argon atmosphere, preserving heat for 5min, and cooling to obtain V2Bulk material of AlC.
Example 3
Microwave sintering synthesis of V2A method of forming a bulk material of AlC comprising the steps of:
a. weighing 2.09g of vanadium powder, 0.66g of aluminum powder and 0.25g of graphite powder according to the molar ratio of V to Al to C =2 to 1.2 to 1, and adding 0.12g of CeF3(4%) as a sintering aid, adding the powder into 5ml of absolute ethyl alcohol, grinding for 30min by using a quartz mortar, and drying in vacuum at 50 ℃ for 5h to obtain a mixed raw material;
b. and (3) pressing the mixed raw materials in a steel grinding tool for 60s under the pressure of 240MPa to form a cylindrical blank.
c. Placing the pressed blank in a microwave sintering device, heating to 1250 ℃ in argon atmosphere, preserving heat for 5min, and cooling to obtain V2Bulk material of AlC.
Example 4
Microwave sintering synthesis of V2A method of forming a bulk material of AlC comprising the steps of:
a. weighing 2.09g of vanadium powder, 0.66g of aluminum powder and 0.25g of graphite powder according to the molar ratio of V to Al to C =2 to 1.2 to 1, and adding 0.06g of CeF3(2%) as a sintering aid, adding the powder into 5ml of absolute ethyl alcohol, grinding for 30min by using a quartz mortar, and drying in vacuum at 50 ℃ for 5h to obtain a mixed raw material;
b. and (3) pressing the mixed raw materials in a steel grinding tool for 60s under the pressure of 240MPa to form a cylindrical blank.
c. Placing the pressed blank in a microwave sintering device, heating to 1250 ℃ under argon atmosphere, preserving heat for 5min, cooling, and grinding in a mortar to obtain V2AlC powder material.
The density and purity results for the bulk V2AlC material produced by the above method are shown in the table below:
| examples | Sintering method | Sintering aid | Density (g/cm)3) | Purity of |
| Comparative example 1 | Pressure-free | Is free of | 3.26 | 65.3% |
| Comparative example 2 | Pressure-free | 2%LaF3 | 3.40 | 73.4% |
| Comparative example 3 | Microwave oven | Is free of | 3.78 | 84.5% |
| Example 1 | Microwave oven | 4%LaF3 | 3.90 | 99.1% |
| Example 2 | Microwave oven | 2%LaF3 | 3.85 | 92.3% |
| Example 3 | Microwave oven | 4%CeF3 | 3.89 | 98.5% |
| Example 4 | Microwave oven | 2%CeF3 | 3.86 | 91.8% |
The analysis of the data in the table shows that V is obtained by adding the sintering aid under the same sintering mode2The purity and density of the AlC block material are improved compared with those of the AlC block material without the sintering aid; likewise, V without addition of sintering aid2The purity and density of the AlC block material are improved when the microwave heating is compared with the pressureless heating; under the microwave heating condition, the larger the adding amount of the sintering aid is, the V2The higher the purity and density of AlC bulk material, under the microwave condition, 4% LaF is added3When, V2Bulk AlC materials have the highest purity and density. High purity and high density V2Bulk AlC material in wear resistant material and V2The precursor material of the C two-dimensional material has wide application.
Preparation V prepared according to the above method2The AlC bulk material was tested by X-ray diffraction, scanning electron microscopy and analyzed as follows:
FIG. 1 shows the molar ratio of V: Al: C =2:1.2:1 in example 1, with 4% LaF added3As a sintering aid, X-ray diffraction after pressing under 240MPa and sintering at 1250 ℃ by a microwave sintering method. Almost no impurity peak, which shows that this example can successfully synthesize V with higher purity2AlC。
FIG. 2 shows the synthesis of V under different process conditions2Bulk AlC material, FIG. 2 (a) is V synthesized in comparative example 2 without pressureless addition of sintering aid2Bulk AlC material with more impurity peaks and V2The diffraction peak intensity of AlC is not high, indicating that V is obtained under no-pressure conditions2The AlC bulk material has various impurity types and low purity; FIG. 2 (b) is a graph showing V synthesized in comparative example 3 under microwave conditions without adding a sintering aid2AlC, impurity peak reduced, but diffraction intensity of peak still not high, indicating that V is obtained in the absence of microwave sintering aid2The AlC bulk material has few impurity species and low purity; FIG. 2 (c) (d) is a graph of V synthesized in example 3 and example 1 under microwave conditions with 4% sintering aid added2AlC, almost no impurity peak, and V2Diffraction of AlCThe peak intensity is obviously enhanced, which shows that V is obtained under the condition of adding sintering aid by microwave2The AlC block material has less impurity species and high purity.
FIG. 3 shows the molar ratio of V: Al: C =2:1.2:1 in example 1, with 4% LaF added3As a sintering aid, after being pressed under 240MPa pressure, a scanning electron microscope image of the sintering material sintered at 1250 ℃ by a microwave sintering method can obviously observe strip V through the scanning electron microscope image2AlC crystal grains are fine, the microstructure is uniform, and a complete layered structure is formed.
Claims (10)
1. Microwave sintering synthesis V2The method for preparing the AlC bulk material is characterized by comprising the following steps of:
a. adding vanadium powder, aluminum powder, graphite powder and sintering aid into absolute ethyl alcohol, grinding, uniformly mixing, and vacuum drying to obtain a mixed raw material; the sintering aid is rare earth fluoride;
b. pressing the mixed raw materials into a blank in a mould;
c. placing the blank body in a microwave sintering device, heating in inert atmosphere, and then cooling to room temperature to obtain V2Bulk material of AlC.
2. Microwave sintered synthetic V according to claim 12The method for preparing the AlC bulk material is characterized by comprising the following steps: the sintering aid is LaF3Or CeF3。
3. Microwave sintered synthetic V according to claim 22The method for preparing the AlC bulk material is characterized by comprising the following steps: the molar ratio of the vanadium powder to the aluminum powder to the graphite powder is V to Al to C =2 (1.1-1.4) to 1, and the sintering aid accounts for 2% -4% of the sum of the mass of the vanadium powder, the mass of the aluminum powder and the mass of the graphite powder.
4. Microwave sintered synthetic V according to claim 22The method for preparing the AlC bulk material is characterized by comprising the following steps: the reaction conditions of the microwave sintering are that the microwave sintering frequency is 2.45GHz and the power is 900W.
5. Microwave sintered synthetic V according to claim 42The method for preparing the AlC bulk material is characterized by comprising the following steps: and in the step a, grinding for 30min by using a quartz mortar in a mixing mode.
6. Microwave sintered synthetic V according to claim 52The method for preparing the AlC bulk material is characterized by comprising the following steps: the vacuum drying temperature in the step a is 50 ℃.
7. Microwave sintered synthetic V according to claim 62The method for preparing the AlC bulk material is characterized by comprising the following steps: in the step c, the heating rate of the microwave heating is 100 ℃/min, the temperature is kept for 5min when the temperature is raised to 1250 ℃, and the inert atmosphere is argon.
8. Microwave sintered synthetic V according to claim 72The method for preparing the AlC bulk material is characterized by comprising the following steps: and c, pressing the die in the step b at the pressure of 240MPa for 60 s.
9. V prepared by the process of any one of claims 1 to 82Bulk material of AlC.
10. V according to claim 92AlC bulk material as wear resistant material and V2C precursor material of two-dimensional material.
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| RU2792036C1 (en) * | 2022-11-08 | 2023-03-15 | Федеральное государственное бюджетное учреждение науки Институт структурной макрокинетики и проблем материаловедения им. А.Г. Мержанова Российской академии наук | METHOD OF OBTAINING VANADIUM-ALUMINUM CARBIDE V2AlC USING SELF-PROPAGATING HIGH-TEMPERATURE SYNTHESIS |
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