CN115353395A - Preparation of Ti 2 AlC/B 4 Method for preparing C complex phase ceramic - Google Patents

Preparation of Ti 2 AlC/B 4 Method for preparing C complex phase ceramic Download PDF

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CN115353395A
CN115353395A CN202211161309.XA CN202211161309A CN115353395A CN 115353395 A CN115353395 A CN 115353395A CN 202211161309 A CN202211161309 A CN 202211161309A CN 115353395 A CN115353395 A CN 115353395A
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powder
alc
complex phase
ceramic
preparing
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CN115353395B (en
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朱春城
姜久兴
朱斯宇
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Harbin Shinkansen Rail Transit Technology Co ltd
Harbin Normal University
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Harbin Shinkansen Rail Transit Technology Co ltd
Harbin Normal University
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Abstract

Preparation of Ti 2 AlC/B 4 A method for preparing C complex phase ceramics, which relates to a method for preparing complex phase ceramics. The invention aims to solve the problems that the brittleness of boron carbide and the sintering mechanism of pure B4C ceramic are bulk diffusion and grain boundary diffusion, so that the grain boundary moving resistance is high and the sintering is difficult to compact. The method comprises the steps of firstly, preparing ceramic powder by adopting a self-propagating combustion method; and step two, adopting a hot-pressing sintering process to densify the prepared ceramic powder, so as to prepare the high-density block material. The invention belongs to the field of powder metallurgy.

Description

Preparation of Ti 2 AlC/B 4 Method for preparing C complex phase ceramic
Technical Field
The invention relates to a method for preparing complex phase ceramics, belonging to the field of powder metallurgy.
Background
Mn +1AXn (M is a transition metal, A is a main group element, X is C or N, N = 1)-3, MAX phase for short) phase ceramic is discovered in 1967, and is named MAX phase ternary ceramic for the first time in 2000, and is a structural/functional integrated material with dual characteristics of metal and ceramic. Ti (titanium) 2 AlC, a MAX phase ceramic, combines many of the excellent properties of metals and ceramics, such as electrical conductivity, thermal shock resistance, processability, as well as high thermal stability and good oxidation resistance, making it one of the ideal materials for the production of high temperature engines. High purity Ti compared with other ceramics 2 AlC ceramics are more difficult to synthesize, often accompanied by a certain amount of secondary phase products such as TiC, which somewhat limits their application as high temperature structural materials. Thus, how to prepare high purity Ti 2 The improvement of the performance of AlC ceramic powder by adding a hard second phase composite material has become a new research hotspot.
Boron carbide (B4C) has the characteristics of low density, high melting point, high hardness (second to diamond and boron nitride), high modulus, strong wear resistance, good oxidation resistance, good thermal stability, good acid corrosion resistance, excellent neutron absorption performance and the like, and is considered to be one of the most application potential advanced structural ceramic materials. Because of high hardness of boron carbide, the boron carbide has strong defense capability against kinetic energy bullets and ammunition fragments, and the boron carbide has light weight, so the boron carbide is an ideal material for preparing body armor and protective armor and has attracted wide attention. However, due to the brittleness of boron carbide and the sintering mechanism of pure B4C ceramics being bulk diffusion and grain boundary diffusion, the grain boundary moving resistance is large, and sintering densification is difficult, which affects the application of the boron carbide in the bulletproof field.
At present, in addition to improving a sintering mechanism and a sintering process, the toughness of the boron carbide ceramic is improved, and what is important is to select a second-phase material to be added into the boron carbide ceramic, improve the performance of the composite material through second-phase toughening, improve the toughness of the whole composite material on the premise of ensuring the inherent performance of the boron carbide ceramic, and provide favorable conditions for the specific application of the materials; in order to solve the brittle failure problem of the B4C ceramic, high-purity Ti2AlC ceramic with excellent performance is selectively introduced to prepare the Ti2AlC/B4C complex-phase ceramic. The addition of the second phase Ti2AlC ceramic can be carried out at a lower sintering temperature, so that the growth of B4C crystal grains can be effectively inhibited, and meanwhile, the interface combination between the Ti2AlC and the B4C is strengthened through the Ti2AlC layered structure, so that the aim of improving the toughness of the boron carbide complex phase ceramic is fulfilled.
Disclosure of Invention
The invention aims to solve the problems that the brittleness of boron carbide and the sintering mechanism of pure B4C ceramic are bulk diffusion and grain boundary diffusion, the grain boundary moving resistance is large, and sintering is difficult to compact, and further provides a method for preparing Ti 2 AlC/B 4 C, a method for preparing the composite ceramic.
The technical scheme adopted by the invention for solving the problems is as follows: the method comprises the following specific steps:
step one, preparing ceramic powder by adopting a self-propagating combustion method;
and step two, adopting a hot-pressing sintering process to densify the prepared ceramic powder, so as to prepare the high-density block material.
Further, the step of preparing the ceramic powder by the self-propagating combustion method in the step one is as follows:
step A, putting Ti powder, aluminum powder and graphite powder into a mixing tank, carrying out wet mixing by using absolute ethyl alcohol, wherein the volume of the absolute ethyl alcohol is not more than two thirds of the volume of the mixing tank, the volume of the Ti powder, the aluminum powder and the graphite powder is not more than one half of the volume of the mixing tank, mixing balls by using boron carbide, wherein the mass ratio of the balls is 1;
step B, taking the mixed powder out of the vacuum oven, filling the powder into a rubber sheathed bag in a loose loading manner, continuously compacting the powder, and sealing and compacting the bag after the relative density of the formed green body is 30 percent;
step C, placing the rubber bag filled with the powder into a vacuum negative pressure tank, vacuumizing the equipment to perform cold isostatic pressing;
d, taking the powder blank subjected to vacuum isostatic pressing out of the rubber packing sleeve, putting the powder blank into a combustion synthesis reaction device, vacuumizing and filling argon for 2 times, igniting by using an ignition agent to perform a combustion synthesis reaction, and finishing the combustion reaction within 15-30 seconds to obtain the Ti-containing material with Ti content 2 AlC ceramics;
step E, crushing the ceramic obtained by combustion synthesis on a crusher to obtain particles with the particle size of about 1mm, washing and drying the particles after acid cleaning, and finally grinding the particles into 10-40 mu mTi by a jet mill 2 And (4) AlC powder.
Further, the molar ratio of the Ti powder, the aluminum powder and the graphite in the step A is (2-3.0): (1.0-2.2): 1; the purity of Ti powder is 99.9%, and the particle size is 40 μm; the purity of the aluminum powder is 99.99 percent, and the particle size is 20 mu m; the purity of the graphite powder was 99.99%, and the particle size was 40 μm.
Further, in the step B, the diameter of the rubber sheath is 5cm, and the powder filling height is 15cm.
And further, in the step C, controlling the negative pressure to be not more than-50 kpa, and keeping the pressure for 5-10 min.
And furthermore, the washing solution used in the acid washing in the step E is mixed solution of hydrochloric acid and dilute nitric acid.
Further, in the second step, the hot-pressing sintering process is adopted to densify the prepared ceramic powder, and the specific steps for preparing the high-density block material are as follows:
step a, mixing materials: weighing the Ti prepared in the step one 2 AlC powder and B 4 C, mixing, dry-mixing in a ball mill after mixing, screening the mixed raw materials, and putting the screened raw materials into a vacuum oven for drying for later use;
step b, forming: b, putting the mixed raw materials in the step a into a steel die, and prepressing and molding on a dry powder automatic molding hydraulic machine;
step c, sintering: placing the formed raw material blank into a graphite mould in a vacuum hot-pressing sintering furnace, and obtaining Ti by adopting a two-stage hot-pressing sintering process and a two-stage heating and heat preservation method 2 AlC/B 4 C complex phase ceramic material.
Further, in the step a, the material-ball ratio of the ball mill is 1.
Further, in the step b, the inner diameter of the steel film die is 80mm, the pressure applied by the automatic forming hydraulic machine is 3-5 MPa, the relative density of the formed blank is 55%, and the height of the blank is 50mm.
Furthermore, in the step c, the heating rate of the first stage of the two-stage hot-pressing sintering process and the two-stage heating and heat-preserving method is 5-15 ℃/min, the temperature is 400-600 ℃, the pressure is 40-80 MPa, and the heat-preserving and pressure-preserving time is 1.0-2.0 h; the temperature rise rate of the second stage is 10-25 ℃/min, the temperature is 1000-1800 ℃, the pressure is 40-80 MPa, and the heat preservation and pressure maintaining time is 2.0-2.5 h.
The beneficial effects of the invention are: the invention has the advantages of simple and convenient powder preparation process, rapidness, energy conservation and low cost, the blank body is pressed by adopting a vacuum isostatic pressing method, the uniformity of combustion waves and the stability of combustion speed of powder in the combustion synthesis process are facilitated, the purity of the ternary ceramic powder prepared by the method reaches up to 99.8 percent, and Ti prepared by adopting a special hot pressing process is high 2 AlC/B 4 High compactness, high purity, high yield and layered Ti of C complex phase ceramic 2 The addition of AlC ceramic improves B 4 The toughness of the C ceramic enables the complex phase ceramic to have excellent mechanical properties, and the complex phase ceramic has wide application prospects when used as an anti-striking and anti-impact material.
Drawings
FIG. 1 is Ti 2 XRD schematic diagram of AlC ceramic powder;
FIG. 2 is Ti 2 AlC/B 4 XRD schematic diagram of the C complex phase ceramic;
FIG. 3 is Ti 2 AlC/B 4 XRD schematic diagram of the C complex phase ceramic;
FIG. 4 is Ti 2 AlC/B 4 C, a schematic drawing of a complex phase ceramic SEM scanning electron microscope;
FIG. 5 is Ti 2 AlC/B 4 C, a schematic drawing of a complex phase ceramic SEM scanning electron microscope;
FIG. 6 is an energy spectrum of the present invention.
Detailed Description
The first embodiment is as follows: this embodiment will be described with reference to FIGS. 1 to 6, and one of the methods of the present embodiment for preparing Ti 2 AlC/B 4 The method for preparing the C complex phase ceramic is realized by the following steps:
step one, preparing ceramic powder by adopting a self-propagating combustion method;
and step two, adopting a hot-pressing sintering process to densify the prepared ceramic powder, so as to prepare the high-density block material.
The second embodiment is as follows: this embodiment will be described with reference to FIGS. 1 to 6, and one of the methods of the present embodiment for preparing Ti 2 AlC/B 4 The self-propagating combustion method for preparing ceramic powder in the first step of the C complex phase ceramic preparation method comprises the following steps:
step A, putting Ti powder, aluminum powder and graphite powder into a mixing tank, carrying out wet mixing by using absolute ethyl alcohol, wherein the volume of the absolute ethyl alcohol is not more than two thirds of the volume of the mixing tank, the volume of the Ti powder, the aluminum powder and the graphite powder is not more than one half of the volume of the mixing tank, mixing balls by using boron carbide, wherein the mass ratio of the balls is 1;
b, taking the mixed powder out of the vacuum oven, filling the powder into a rubber sheath bag in a loose loading manner, continuously compacting the powder, and sealing and compacting an opening of the bag, wherein the relative density of the molded blank is 30%;
step C, placing the rubber bag filled with the powder into a vacuum negative pressure tank, vacuumizing the equipment, and carrying out cold isostatic pressing;
d, taking the powder blank subjected to vacuum isostatic pressing out of the rubber packing sleeve, putting the powder blank into a combustion synthesis reaction device, vacuumizing and filling argon for 2 times, igniting by using an ignition agent to perform a combustion synthesis reaction, and finishing the combustion reaction within 15-30 seconds to obtain the Ti-containing material with Ti content 2 AlC ceramics;
step E, crushing the ceramic obtained by combustion synthesis on a crusher to obtain particles with the particle size of about 1mm, pickling the particles, cleaning and dryingDrying, and grinding into 10-40 μmTi with jet mill 2 AlC powder.
The third concrete implementation mode: this embodiment will be described with reference to FIGS. 1 to 6, which illustrate a method for preparing Ti 2 AlC/B 4 C, in the step A of the method for multiphase ceramics, the molar ratio of the Ti powder, the aluminum powder and the graphite is (2-3.0): (1.0-2.2): 1; the purity of Ti powder is 99.9%, and the particle size is 40 μm; the purity of the aluminum powder is 99.99 percent, and the particle size is 20 mu m; the purity of the graphite powder was 99.99%, and the particle size was 40 μm.
The fourth concrete implementation mode: this embodiment will be described with reference to FIGS. 1 to 6, and one of the methods of the present embodiment for preparing Ti 2 AlC/B 4 And C, in the step B of the method for multiphase ceramics, the diameter of the rubber sheath is 5cm, and the powder filling height is 15cm.
The fifth concrete implementation mode: this embodiment will be described with reference to FIG. 1, which illustrates one method of preparing Ti 2 AlC/B 4 C, controlling the negative pressure not more than-50 kpa in the step C of the complex phase ceramic method, and keeping the pressure for 5-10 min.
The sixth specific implementation mode: this embodiment will be described with reference to FIGS. 1 to 6, and one of the methods of the present embodiment for preparing Ti 2 AlC/B 4 And C, the washing liquid used in the acid washing in the step E of the method for multiphase ceramics is mixed solution of hydrochloric acid and dilute nitric acid.
The seventh concrete implementation mode: this embodiment will be described with reference to FIGS. 1 to 6, and one of the methods of the present embodiment for preparing Ti 2 AlC/B 4 Step two of the method for preparing the complex phase ceramic adopts a hot-pressing sintering process to densify the prepared ceramic powder, and the specific steps for preparing the high-density block material are as follows:
step a, mixing materials: weighing the Ti prepared in the step one 2 AlC powder and B 4 C, mixing, dry-mixing in a ball mill, sieving the mixed raw materials, and drying in a vacuum oven for later use;
step b, forming: b, putting the mixed raw materials in the step a into a steel die, and prepressing and molding on a dry powder automatic molding hydraulic machine;
step c, sintering: putting the molded raw material blank into vacuumIn a graphite mould in a hot-pressing sintering furnace, ti is obtained by adopting a two-stage hot-pressing sintering process and a two-stage heating and heat preservation method 2 AlC/B 4 C complex phase ceramic material.
The specific implementation mode is eight: this embodiment will be described with reference to FIGS. 1 to 6, and one of the methods of the present embodiment for preparing Ti 2 AlC/B 4 In the step a of the method for the composite phase ceramic, the material-ball ratio in a ball mill is 1 to 5, the dry mixing time is 12 to 24 hours, the rotating speed of the ball mill is 100 to 300r/min, and the temperature in a vacuum oven is 60 ℃.
The specific implementation method nine: this embodiment will be described with reference to FIGS. 1 to 6, which illustrate a method for preparing Ti 2 AlC/B 4 And C, in the step b of the method of the complex phase ceramics, the inner diameter of the steel film die is 80mm, the pressure applied by the automatic molding hydraulic press is 3-5 MPa, the relative density of the molded blank is 55%, and the height of the blank is 50mm.
The specific implementation mode is ten: this embodiment will be described with reference to FIGS. 1 to 6, and one of the methods of the present embodiment for preparing Ti 2 AlC/B 4 C, in the step C of the complex phase ceramic method, the heating rate of the two-stage hot pressing sintering process and the first stage of the two-stage heating and heat preservation method is 5-15 ℃/min, the temperature is 400-600 ℃, the pressure is 40-80 MPa, and the heat preservation and pressure maintaining time is 1.0-2.0 h; the temperature rise rate of the second stage is 10-25 ℃/min, the temperature is 1000-1800 ℃, the pressure is 40-80 MPa, and the heat preservation and pressure maintaining time is 2.0-2.5 h.
Examples
Preparation of high-purity Ti by self-propagating combustion method 2 AlC ceramic powder examples
Example 1
Step one, carrying out wet mixing on Ti powder (the average particle size is less than or equal to 45 microns, the purity is more than 99.9%), aluminum powder (the average particle size is less than or equal to 20 microns, and the purity is more than 99.99%) and graphite powder (the average particle size is less than or equal to 40 microns, and the purity is 99.99%) according to a molar ratio of 2;
step two, putting a certain weight of mixed powder into a rubber wrapping bag with the diameter of 5cm, compacting and sealing the powder, putting the rubber wrapping bag filled with the powder into a vacuum negative pressure tank, controlling the negative pressure to be below-50 kpa, keeping the pressure for 5min, and carrying out cold isostatic pressing;
step three, taking the blank after vacuum isostatic pressing out of the rubber bag sleeve, putting the blank into a combustion synthesis reaction device, vacuumizing and filling argon for 2 times, igniting by using an ignition agent to perform combustion synthesis reaction, and completing the combustion reaction in about 15 seconds to obtain Ti with certain compactness 2 AlC ceramic powder;
and step four, crushing the ceramic obtained by combustion synthesis on a crusher (a jaw crusher, model 100 x 60) to obtain particles with the particle size of about 1mm, washing and drying the particles after acid washing (hydrochloric acid and diluted nitric acid), and finally grinding the particles into powder with the particle size of 10 microns by using an air flow mill.
Example 2
Step one, wet mixing Ti powder (the average particle size is less than or equal to 45 microns, the purity is more than 99.9%), aluminum powder (the average particle size is less than or equal to 20 microns, and the purity is more than 99.99%) and graphite powder (the average particle size is less than or equal to 40 microns, and the purity is 99.99%) according to a molar ratio of 2.5;
step two, putting a certain weight of mixed powder into a rubber wrapping bag with the diameter of 5cm, compacting and sealing the powder, putting the rubber wrapping bag filled with the powder into a vacuum negative pressure tank, controlling the negative pressure to be below-50 kpa, keeping the pressure for 5min, and carrying out cold isostatic pressing;
step three, taking the blank after vacuum isostatic pressing out of the rubber bag sleeve, putting the blank into a combustion synthesis reaction device, vacuumizing and filling argon for 2 times, igniting by using an ignition agent to perform combustion synthesis reaction, and completing the combustion reaction in about 15 seconds to obtain Ti with certain compactness 2 AlC ceramic powder;
and step four, crushing the ceramic obtained by combustion synthesis on a crusher (a jaw crusher, model 100 x 60) to obtain particles with the particle size of about 1mm, washing and drying the particles after acid washing (hydrochloric acid and diluted nitric acid), and finally grinding the particles into powder with the particle size of 10 microns by using an air jet mill.
Example 3
Step one, carrying out wet mixing on Ti powder (the average particle size is less than or equal to 45 microns, the purity is more than 99.9%), aluminum powder (the average particle size is less than or equal to 20 microns, and the purity is more than 99.99%) and graphite powder (the average particle size is less than or equal to 40 microns, and the purity is 99.99%) according to a molar ratio of 2;
step two, putting a certain weight of mixed powder into a rubber wrapping bag with the diameter of 5cm, compacting and sealing the powder, putting the rubber wrapping bag with the powder into a vacuum negative pressure tank, controlling the negative pressure to be below-50 kpa, keeping the pressure for 5min, and carrying out cold isostatic pressing;
step three, taking the blank after vacuum isostatic pressing out of the rubber bag sleeve, putting the blank into a combustion synthesis reaction device, vacuumizing and filling argon for 2 times, igniting by using an ignition agent to perform combustion synthesis reaction, and completing the combustion reaction in about 15 seconds to obtain Ti with certain compactness 2 AlC ceramic powder;
and step four, crushing the ceramic obtained by combustion synthesis on a crusher (a jaw crusher, model 100 x 60) to obtain particles with the particle size of about 1mm, washing and drying the particles after acid washing (hydrochloric acid and diluted nitric acid), and finally grinding the particles into powder with the particle size of 10 microns by using an air flow mill.
Comparative examples 1, 2 and 3 raw material ratios
The preparation methods of examples 1, 2 and 3 are basically the same, except that the molar ratio of the Ti powder, the aluminum powder and the graphite powder is selected from the following ratio of "2;
comparative examples 1, 2, 3 test for purity of materials
Ti prepared in examples 1, 2 and 3 2 The XRD pattern of AlC ceramic powder is shown in FIG. 1. As can be seen from FIG. 1, ti prepared by the present invention 2 All the AlC ceramic powders have higher purity, but the Ti prepared by the method of example 2 2 The purity of AlC powder is highest, basically no impurities are contained, and the purity is close to 100 percent, which is the report that Ti is prepared at present 2 Highest purity of AlC.
Preparation of Ti by hot-pressing sintering 2 AlC/B 4 C complex phase ceramic
Example 4
Step one, preparing Ti by a self-propagating combustion method 2 AlC ceramic powder (average grain diameter less than or equal to 10 μm, purity greater than 99.8%), B 4 Mixing C powder (with the average particle size of 10 mu m and the purity of more than 99.9%) according to a weight ratio (wt%) of 1;
step two, weighing the mixed Ti 2 AlC、B 4 300g of the raw material C is put into a steel die mould with the diameter of 80mm, and prepressing and forming are carried out under the pressure of 4 MPa;
putting the prepressed molded blank into a vacuum hot-pressing sintering furnace, and performing hot-pressing sintering by adopting a two-stage heating process under a vacuum condition, wherein the first stage comprises the steps of heating at a speed of 10 ℃/min, heating at 600 ℃, keeping the pressure at 50MPa and keeping the temperature and the pressure for 1.5h; the second stage is that the Ti with excellent comprehensive performance is obtained after the temperature rise rate is 15 ℃/min, the temperature is 1300 ℃, the pressure is 70MPa and the heat preservation and pressure maintaining time is 2.0h and then is cooled to the room temperature along with the furnace 2 AlC/B 4 C complex phase ceramic material.
Example 5
Step one, preparing Ti by a self-propagating combustion method 2 AlC ceramic powder (average grain diameter less than or equal to 10 μm, purity greater than 99.8%), B 4 C powder (the average particle size is less than or equal to 10 microns, the purity is more than 99.9%) is prepared according to the weight ratio (wt%) of 5;
step two, weighing the mixed Ti 2 AlC、B 4 300g of the C powder raw material is put into a steel die mould with the diameter of 80mm and is pre-pressed and formed under the pressure of 4 MPa;
thirdly, putting the pre-pressed and molded blank into a vacuum hot-pressing sintering furnace, and performing hot-pressing sintering by adopting a two-stage heating process under a vacuum condition, wherein the first stage comprises the steps of heating at a speed of 10 ℃/min, heating at a temperature of 850 ℃, keeping the pressure at 50MPa and keeping the temperature and the pressure for 2.0h;the second stage is that the Ti with excellent comprehensive performance is obtained after the temperature rise rate is 15 ℃/min, the temperature is 1800 ℃, the pressure is 80MPa and the heat preservation and pressure maintaining time is 2.0h and the Ti is cooled to the room temperature along with the furnace 2 AlC/B 4 C complex phase ceramic material.
Example 6
Step one, preparing Ti by a self-propagating combustion method 2 AlC ceramic powder (average grain diameter less than or equal to 10 μm, purity greater than 99.8%), B 4 C, mixing powder (the average particle size is less than or equal to 10 microns, the purity is more than 99.9%) according to a weight ratio (wt%) of 10;
step two, weighing the mixed Ti 2 AlC、B 4 300g of the C powder raw material is put into a steel die mould with the diameter of 80mm and is pre-pressed and formed under the pressure of 4 MPa;
thirdly, putting the pre-pressed molded blank into a vacuum hot-pressing sintering furnace, and performing hot-pressing sintering by adopting a two-stage heating process under a vacuum condition, wherein the first stage comprises the steps of heating at a speed of 10 ℃/min, heating at a temperature of 800 ℃, keeping the pressure at 50MPa and keeping the temperature and the pressure for 2.0h; the second stage is that the Ti with excellent comprehensive performance is obtained after the temperature rise rate is 15 ℃/min, the temperature is 1450 ℃, the pressure is 75MPa and the heat preservation and pressure maintaining time is 2.0h and the Ti is cooled to the room temperature along with the furnace 2 AlC/B 4 C complex phase ceramic material.
All Ti of the invention is obtained by XRD and scanning electron microscope 2 AlC/B 4 C phase composition and morphology characteristics of the complex phase ceramic, and results show that all prepared materials meet the intrinsic characteristic requirements.
TABLE 1 Ti 2 AlC/B 4 Purity and performance of C complex phase ceramic
Figure BDA0003860108400000081
Although the present invention has been described with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the present invention.

Claims (10)

1. Preparation of Ti 2 AlC/B 4 The method for C complex phase ceramics is characterized in that: the preparation of Ti 2 AlC/B 4 The method for preparing the C complex phase ceramic is realized by the following steps:
step one, preparing ceramic powder by adopting a self-propagating combustion method;
and step two, adopting a hot-pressing sintering process to densify the prepared ceramic powder, so as to prepare the high-density block material.
2. A process for preparing Ti according to claim 1 2 AlC/B 4 The method for C complex phase ceramics is characterized in that: the method for preparing the ceramic powder by the self-propagating combustion method in the first step comprises the following steps:
step A, putting Ti powder, aluminum powder and graphite powder into a mixing tank, carrying out wet mixing by using absolute ethyl alcohol, wherein the volume of the absolute ethyl alcohol is not more than two thirds of the volume of the mixing tank, the volume of the Ti powder, the aluminum powder and the graphite powder is not more than one half of the volume of the mixing tank, mixing balls by using boron carbide, wherein the mass ratio of the balls is 1;
b, taking the mixed powder out of the vacuum oven, filling the powder into a rubber sheath bag in a loose loading manner, continuously compacting the powder, and sealing and compacting an opening of the bag, wherein the relative density of the molded blank is 30%;
step C, placing the rubber bag filled with the powder into a vacuum negative pressure tank, vacuumizing the equipment to perform cold isostatic pressing;
d, taking the powder blank subjected to vacuum isostatic pressing out of the rubber packing sleeve, putting the powder blank into a combustion synthesis reaction device, vacuumizing and filling argon for 2 times, igniting by using an ignition agent to perform a combustion synthesis reaction, and finishing the combustion reaction within 15-30 seconds to obtain the Ti-containing material with Ti content 2 AlC ceramics;
step E, crushing the ceramic obtained by combustion synthesis on a crusher to obtain particles with the particle size of about 1mm, washing and drying the particles after acid cleaning, and finally grinding the particles into 10-40 mu mTi by a jet mill 2 AlC powder.
3. A method of producing Ti according to claim 2 2 AlC/B 4 The method for C complex phase ceramics is characterized in that: the molar ratio of the Ti powder, the aluminum powder and the graphite in the step A is (2-3.0): (1.0-2.2): 1; the purity of Ti powder is 99.9%, and the particle size is 40 μm; the purity of the aluminum powder is 99.99 percent, and the particle size is 20 mu m; the purity of the graphite powder is 99.99%, and the particle size is 40 μm.
4. A method of producing Ti according to claim 2 2 AlC/B 4 The method for C complex phase ceramics is characterized in that: in the step B, the diameter of the rubber sheath is 5cm, and the powder filling height is 15cm.
5. A method of producing Ti according to claim 2 2 AlC/B 4 The method for C complex phase ceramics is characterized in that: and C, controlling the negative pressure not to be more than-50 kpa, and keeping the pressure for 5-10 min.
6. A method of producing Ti according to claim 2 2 AlC/B 4 The method for C complex phase ceramics is characterized in that: and E, washing liquor used in the acid washing in the step E is mixed liquor of hydrochloric acid and dilute nitric acid.
7. A process for preparing Ti according to claim 1 2 AlC/B 4 The method for C complex phase ceramics is characterized in that: in the second step, the ceramic powder is densified by adopting a hot-pressing sintering process to prepare a high-density blockThe specific steps of the material are as follows:
step a, mixing materials: weighing the Ti prepared in the step one 2 AlC powder and B 4 C, mixing, dry-mixing in a ball mill after mixing, screening the mixed raw materials, and putting the screened raw materials into a vacuum oven for drying for later use;
step b, forming: b, putting the mixed raw materials in the step a into a steel die, and prepressing and molding on a dry powder automatic molding hydraulic machine;
step c, sintering: placing the formed raw material blank into a graphite mould in a vacuum hot-pressing sintering furnace, and obtaining Ti by adopting a two-stage hot-pressing sintering process and a two-stage heating and heat preservation method 2 AlC/B 4 C complex phase ceramic material.
8. The method of claim 7, wherein the Ti is prepared by 2 AlC/B 4 The method for C complex phase ceramics is characterized in that: in the step a, the material-ball ratio in the ball mill is 1.
9. The method of claim 7, wherein the Ti is prepared by 2 AlC/B 4 The method for C complex phase ceramics is characterized in that: in the step b, the inner diameter of the steel film die is 80mm, the pressure applied by the automatic forming hydraulic press is 3-5 MPa, the relative density of the formed blank is 55%, and the height of the blank is 50mm.
10. A method of preparing Ti according to claim 7 2 AlC/B 4 The method for C complex phase ceramics is characterized in that: in the step c, the heating rate of the first stage of the two-stage hot-pressing sintering process and the two-stage heating and heat preservation method is 5-15 ℃/min, the temperature is 400-600 ℃, the pressure is 40-80 MPa, and the heat preservation and pressure maintaining time is 1.0-2.0 h; the temperature rise rate of the second stage is 10-25 ℃/min, the temperature is 1000-1800 ℃, the pressure is 40-80 MPa, and the heat preservation and pressure maintaining time is 2.0-2.5 h.
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WO2016016169A1 (en) * 2014-07-28 2016-02-04 Centre De Transfert De Technologies Ceramiques (C.T.T.C.) Composite material for an anti-ballistic protection device comprising ceramic objects in a binder matrix and method for producing such a material

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Publication number Priority date Publication date Assignee Title
CN101037334A (en) * 2007-04-27 2007-09-19 武汉理工大学 Compact Ti2AlC-TiB2 composite material and preparation method therefor
CN101037201A (en) * 2007-04-27 2007-09-19 武汉理工大学 High-purity Ti2AlC powder material and preparing method thereof
CN101186294A (en) * 2007-12-12 2008-05-28 哈尔滨工业大学 Method of preparing high purity Ti2AlC block material
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