CN110655408B - Preparation method of single-phase carborundum solid solution ceramic material - Google Patents
Preparation method of single-phase carborundum solid solution ceramic material Download PDFInfo
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Abstract
The invention relates to a preparation method of a single-phase carborundum solid solution ceramic material, belonging to the technical field of superhard ceramic materials. The application solves the problems that the prior transition metal carbide and boride have lower solid solubility and are difficult to prepare and obtain the transition metal carbide and boride. The invention adopts a high-energy ball milling mode to prepare the transition metal carbide and the boride into composite powder, and then adopts a discharge plasma sintering or hot-pressing sintering mode to prepare the superhard boride ceramic sintered body. The method can widen the solid solubility limit of carbide in boride by using high-energy ball milling, solves the problem of low solid solubility between transition metal carbide and boride, and obviously improves the strength and hardness of a sintered body by the solid solution strengthening effect between ball-milled composite powder; meanwhile, the high-energy ball milling enables the particle size of the powder to be refined, and the sintering temperature can be effectively reduced.
Description
Technical Field
The invention relates to a preparation method of a single-phase carborundum solid solution ceramic material, belonging to the technical field of superhard ceramic materials.
Background
The superhard material has wide application in the aspects of abrasive materials, cutting tools, wear-resistant coatings and the like. Ballistic armor ceramics that have been investigated in recent years have also placed high demands on the hardness of the material. The hardest material known in nature is diamond, which is expensive and difficult to machine into complex shapes. The hardness of cubic boron nitride (c-BN) in common ceramic materials is the highest and exceeds 50 GPa. Boron carbide (B)4C) And their composites also have high hardness, typically exceeding 30 GPa. But c-BN and B4C belongs to a compound with strong covalent bond, the self-diffusion coefficient in the sintering process is very low, and the material is difficult to sinter and form. Furthermore, c-BN and B4Of material CPoor toughness, generally less than 3MPa m1/2Limiting its application.
Transition metal borides (e.g. TiB)2，ZrB2，HfB2Etc.) hardness lower than c-BN and B4C, but it can be 20GPa or more. And the carbide is added into the single-phase boride to be used as an oxygen scavenger, so that the sintering temperature of the material can be reduced, and the densification is promoted. But TiB2，ZrB2，HfB2The crystal structure of the boride is a hexagonal structure, while the crystal structure of the transition metal carbide is a NaCl profile surface-centered cubic structure, and the boride and the crystal are difficult to form a single-phase boride solid solution ceramic material in a solid solution manner under normal conditions. Therefore, it is necessary to provide a method for preparing single-phase boride solid solution ceramic material.
Disclosure of Invention
The invention provides a preparation method of a superhard single-phase carborundum quaternary solid solution ceramic material, aiming at solving the problems that the existing transition metal carbide and boride have lower solid solubility and are difficult to prepare and obtain the transition metal carborundum.
The technical scheme of the invention is as follows:
a preparation method of the single-phase carborundum solid solution ceramic material comprises the following steps:
mixing boride-containing powder and carbide-containing powder, and performing ball milling by using a high-energy ball mill to obtain composite powder;
and step two, placing the composite powder subjected to ball milling in the step one in a mould for sintering to obtain the single-phase carborundum solid solution ceramic material.
Preferably: the boron-containing compound is titanium boride, zirconium boride, hafnium boride, niobium boride, tantalum boride, tungsten boride or molybdenum boride.
Most preferably: the carbide-containing substance is titanium carbide, zirconium carbide, hafnium carbide, niobium carbide, tantalum carbide, tungsten carbide or molybdenum carbide.
Most preferably: the metal element in the boron-containing compound and the metal element in the carbon-containing compound are different metal elements.
Preferably: the composite powder contains 70-99% of boride powder and 1-30% of carbide powder by mass.
Preferably: the ball milling conditions of the high-energy ball mill in the first step are as follows: the ball-material ratio is 10-100: 1, the rotating speed is 400-800 r/min, and the ball milling time is 5-40 h.
Preferably: the sintering of the second step is carried out in a discharge plasma furnace, and the sintering conditions are as follows: the sintering temperature is 1800-2300 ℃, the heat preservation time is 5-60 min, the sintering pressure is 30-80 MPa, and the heating rate is 50-150 ℃/min.
Preferably: the sintering in the second step is carried out in a hot pressing furnace, and the sintering conditions are as follows: the sintering temperature is 1800-2300 ℃, the heat preservation time is 0.5-10 h, the sintering pressure is 30-80 MPa, and the heating rate is 10-40 ℃/min.
The invention has the following beneficial effects: the method adopts a high-energy ball milling mode to prepare the transition metal carbide and the boride into composite powder, and then adopts a spark plasma sintering or hot-pressing sintering mode to prepare the superhard boride ceramic sintered body. The method adopts high-energy ball milling to widen the solid solubility limit of carbide in boride, solves the problem of low solid solubility between transition metal carbide and boride, and obviously improves the strength and hardness of a sintered body due to the solid solution strengthening effect between the ball-milled composite powder; meanwhile, the high-energy ball milling enables the particle size of the powder to be refined, and the sintering temperature can be effectively reduced. And by strictly controlling the parameters of the discharge plasma sintering furnace or the hot pressing furnace, the superstrong and high-hardness single-phase boride quaternary solid solution ceramic material is finally obtained.
Drawings
FIG. 1 is a schematic XRD diagram of a ceramic material prepared according to embodiment 1;
fig. 2 is a surface SEM photograph of the ceramic material prepared in embodiment 1.
Detailed Description
The experimental procedures used in the following examples are conventional unless otherwise specified.
Embodiment mode 1: the boride is titanium boride and the carbide is zirconium carbide
(1) Mixing titanium boride powder and zirconium carbide powder according to a mass ratio of 85:15, and ball-milling by using a high-energy ball mill under the following ball-milling conditions: the ball-material ratio is 10:1, the ball milling time is 30h, and the rotating speed is 500r/min, so that composite powder with uniform components and fine particles is obtained;
(2) placing the composite powder in a mould, and sintering in a hot pressing furnace under the following sintering conditions: and (3) heating the graphite heating body in the hot pressing furnace to 2000 ℃ at the speed of 20 ℃/min, carrying out heat preservation sintering for 1h at the sintering pressure of 30Mpa, and cooling and demoulding after sintering to obtain the single-phase carbon boride solid solution ceramic material (i).
XRD testing was performed on the single phase solid solution carbonitride ceramic material (i) and the results are shown in FIG. 1. As can be seen from FIG. 1, after hot-pressing sintering, the material has a diffraction peak shape similar to that of titanium boride, but the angle is shifted to a low angle, and the diffraction peak of zirconium carbide disappears, indicating that a single-phase solid solution is formed.
SEM tests were performed on the surface of the single phase boride solid solution ceramic material (i) and the results are shown in FIG. 2. As can be seen from FIG. 2, the material is composed of a matrix phase and a black impurity phase, wherein the matrix is a single-phase solid solution, the black phase is a carbon residue phase caused by the atmosphere of a graphite furnace, and the material structure is uniform.
The single-phase carborundum solid solution ceramic material (i) is characterized by mechanical properties, and the result shows that the hardness of the material at room temperature is 35 +/-1.3 GPa, the three-point bending strength is 610 +/-23 MPa, the elastic modulus is 510GPa, and the fracture toughness is 4.82 MPa.m1/2. And the density of the single-phase carborundum solid solution ceramic material (i) is 4.63 g-cm3。
Embodiment mode 2: the boride is titanium boride and the carbide is zirconium carbide
(1) Mixing titanium boride powder and zirconium carbide powder according to a mass ratio of 90:10, and ball-milling by using a high-energy ball mill under the following ball-milling conditions: the ball-material ratio is 10:1, the ball milling time is 30h, and the rotating speed is 500r/min, so that composite powder with uniform components and fine particles is obtained;
(2) placing the composite powder in a mould, and sintering in a hot pressing furnace under the following sintering conditions: and (3) heating the graphite heating body in the hot pressing furnace to 2000 ℃ at the speed of 20 ℃/min, carrying out heat preservation sintering for 1h, wherein the sintering pressure is 30Mpa, and cooling and demoulding after sintering to obtain the single-phase carbon boride solid solution ceramic material (ii).
The single-phase carborundum solid solution ceramic material (ii) is characterized by mechanical properties, and the result shows that the hardness of the material at room temperature is 33 +/-1.5 GPa, the three-point bending strength is 572 +/-64 MPa, the elastic modulus is 520GPa, and the fracture toughness is 4.95 MPa.m1/2. And the density of the single-phase carborundum solid solution ceramic material (ii) is 4.46 g-cm3。
Embodiment mode 3: the boride is titanium boride and the carbide is zirconium carbide
(1) Mixing titanium boride powder and zirconium carbide powder according to a mass ratio of 95:5, and ball-milling by using a high-energy ball mill under the following ball-milling conditions: the ball-material ratio is 10:1, the ball milling time is 30h, and the rotating speed is 500r/min, so that composite powder with uniform components and fine particles is obtained;
(2) placing the composite powder in a mould, and sintering in a hot pressing furnace under the following sintering conditions: and (3) heating the graphite heating body in the hot pressing furnace to 2000 ℃ at the speed of 20 ℃/min, carrying out heat preservation sintering for 1h at the sintering pressure of 30Mpa, and cooling and demoulding after sintering to obtain the single-phase carbon boride solid solution ceramic material (iii).
The single-phase carborundum solid solution ceramic material (iii) is characterized by mechanical properties, and the result shows that the hardness of the material at room temperature is 31 +/-2.3 GPa, the three-point bending strength is 544 +/-56 MPa, the elastic modulus is 525GPa, and the fracture toughness is 4.54 MPa.m1/2. And the density of the single-phase carborundum solid solution ceramic material (iii) is 4.29 g-cm3。
Embodiment 4: the boride is titanium boride, and the carbide is niobium carbide
(1) Mixing titanium boride powder and niobium carbide powder according to a mass ratio of 85:15, and carrying out ball milling by using a high-energy ball mill under the ball-material ratio of 20:1, the ball milling time of 20 hours and the rotating speed of 500r/min to obtain composite powder with uniform components and fine particles;
(2) placing the composite powder in a mould, and sintering in a discharge plasma furnace, wherein the sintering conditions are as follows: and (3) heating the discharge plasma furnace to 2000 ℃ at the speed of 100 ℃/min, carrying out heat preservation sintering for 5min, wherein the sintering pressure is 40Mpa, and cooling and demoulding after sintering to obtain the single-phase boride solid solution ceramic material (iiii).
The single-phase carborundum solid solution ceramic material (iiii) is characterized by mechanical properties, and the result shows that the hardness of the material at room temperature is 31 +/-2.4 GPa, the three-point bending strength is 520 +/-16 MPa, the elastic modulus is 520GPa, and the fracture toughness is 5.12 MPa.m1/2. And the density of the single-phase carborundum solid solution ceramic material (iiii) is 4.70 g-cm3。
Embodiment 5: the boride is titanium boride, and the carbide is niobium carbide
(1) Mixing titanium boride powder and niobium carbide powder according to a mass ratio of 90:10, and carrying out ball milling by using a high-energy ball mill under the ball-material ratio of 20:1, the ball milling time of 20h and the rotating speed of 500r/min to obtain composite powder with uniform components and fine particles;
(2) placing the composite powder in a mould, and sintering in a discharge plasma furnace, wherein the sintering conditions are as follows: and (3) heating the discharge plasma furnace to 2000 ℃ at the speed of 100 ℃/min, carrying out heat preservation sintering for 5min, wherein the sintering pressure is 40Mpa, and cooling and demoulding after sintering to obtain the single-phase boride solid solution ceramic material (v).
The single-phase carborundum solid solution ceramic material (v) is characterized by mechanical properties, and the result shows that the hardness of the material at room temperature is 30 +/-3.1 GPa, the three-point bending strength is 418 +/-84 MPa, the elastic modulus is 525GPa, and the fracture toughness is 4.73 MPa.m1/2. And the density of the single-phase carborundum solid solution ceramic material (v) is 4.50 g-cm3。
Embodiment 6: the boride is titanium boride, and the carbide is niobium carbide
(1) Mixing titanium boride powder and niobium carbide powder according to a mass ratio of 95:5, and carrying out ball milling by using a high-energy ball mill under the ball-material ratio of 20:1, the ball milling time of 20h and the rotating speed of 500r/min to obtain composite powder with uniform components and fine particles;
(2) placing the composite powder in a mould, and sintering in a discharge plasma furnace, wherein the sintering conditions are as follows: and (3) heating the discharge plasma furnace to 2000 ℃ at the speed of 100 ℃/min, carrying out heat preservation sintering for 5min, wherein the sintering pressure is 40Mpa, and cooling and demoulding after sintering to obtain the single-phase carborundum solid solution ceramic material (vi).
The single-phase carborundum solid solution ceramic material (vi) is characterized by mechanical properties, and the result shows that the hardness of the material at room temperature is 28 +/-1.6 GPa, the three-point bending strength is 431 +/-55 MPa, the elastic modulus is 528GPa, and the fracture toughness is 3.97 MPa.m1/2. And the density of the single-phase carborundum solid solution ceramic material (v) is 4.32 g-cm3。
Embodiment 7: the boride is titanium boride and the carbide is tantalum carbide
(1) Mixing titanium boride powder and tantalum carbide powder according to a mass ratio of 75:25, and carrying out ball milling by using a high-energy ball mill under the ball-material ratio of 10:1, the ball milling time of 24 hours and the rotating speed of 500r/min to obtain composite powder with uniform components and fine particles;
(2) placing the composite powder in a mould, and sintering in a hot pressing furnace under the following sintering conditions: and (2) heating the graphite heating body in the hot pressing furnace to 2050 ℃ at the speed of 20 ℃/min, carrying out heat preservation sintering for 1h, wherein the sintering pressure is 40Mpa, and cooling and demoulding after sintering to obtain the single-phase carbon boride solid solution ceramic material (vii).
The single-phase carborundum solid solution ceramic material (vii) is characterized by mechanical properties, and as a result, the hardness of the material at room temperature is 30 +/-0.8 GPa, the three-point bending strength is 510 +/-41 MPa, the elastic modulus is 480GPa, and the fracture toughness is 4.08 MPa.m1/2. And the density of the single-phase carborundum solid solution ceramic material (vii) is 5.32 g-cm3。
Embodiment mode 8: the boride is titanium boride and the carbide is tantalum carbide
(1) Mixing titanium boride powder and tantalum carbide powder according to a mass ratio of 85:15, and carrying out ball milling by using a high-energy ball mill under the ball-material ratio of 10:1, the ball milling time of 24 hours and the rotating speed of 500r/min to obtain composite powder with uniform components and fine particles;
(2) placing the composite powder in a mould, and sintering in a hot pressing furnace under the following sintering conditions: and (3) heating the graphite heating body in the hot pressing furnace to 2050 ℃ at the speed of 20 ℃/min, carrying out heat preservation sintering for 1h, wherein the sintering pressure is 40Mpa, and cooling and demoulding after sintering to obtain the single-phase carbon boride solid solution ceramic material (viii).
The single-phase carborundum solid solution ceramic material (viii) is characterized by mechanical properties, and the result shows that the hardness of the material at room temperature is 28 +/-2.4 GPa, the three-point bending strength is 508 +/-11 MPa, the elastic modulus is 501GPa, and the fracture toughness is 4.32 MPa.m1/2. And the density of the single-phase carborundum solid solution ceramic material (viii) is 4.81g cm3。
Embodiment mode 9: the boride is titanium boride and the carbide is tantalum carbide
(1) Mixing titanium boride powder and tantalum carbide powder according to a mass ratio of 95:5, and carrying out ball milling by using a high-energy ball mill under the ball-material ratio of 10:1, the ball milling time of 30h and the rotating speed of 500r/min to obtain composite powder with uniform components and fine particles;
(2) placing the composite powder in a mould, and sintering in a hot pressing furnace under the following sintering conditions: and (3) heating the graphite heating body in the hot pressing furnace to 2050 ℃ at the speed of 20 ℃/min, carrying out heat preservation sintering for 1h, wherein the sintering pressure is 40Mpa, and cooling and demoulding after sintering to obtain the single-phase carbon boride solid solution ceramic material (viii).
The single-phase carborundum solid solution ceramic material (viii) is characterized by mechanical properties, and the surface results show that the hardness of the material at room temperature is 26 +/-1.1 GPa, the three-point bending strength is 432 +/-103 MPa, the elastic modulus is 520GPa, and the fracture toughness is 3.54 MPa.m1/2. And the density of the single-phase carborundum solid solution ceramic material (viii) is 2.98 g-cm3。
Embodiment 10: the boride is titanium boride and the carbide is hafnium carbide
(1) Mixing titanium boride powder and hafnium carbide powder according to a mass ratio of 75:25, and carrying out ball milling by using a high-energy ball mill under the ball-material ratio of 40:1, the ball milling time of 10h and the rotating speed of 500r/min to obtain composite powder with uniform components and fine particles;
(2) placing the composite powder in a mould, and sintering in a hot pressing furnace under the following sintering conditions: heating a graphite heating body in a hot pressing furnace to 2100 ℃ at the speed of 20 ℃/min, carrying out heat preservation sintering for 1h, wherein the sintering pressure is 50Mpa, and cooling and demoulding after sintering to obtain the single-phase boride solid solution ceramic material (vv).
The single-phase carborundum solid solution ceramic material (vv) is characterized by mechanical properties, and the result shows that the hardness of the material at room temperature is 30 +/-0.7 GPa, the three-point bending strength is 550 +/-7 MPa, the elastic modulus is 505GPa, and the fracture toughness is 4.13 MPa.m1/2. And the density of the single-phase carborundum solid solution ceramic material (vv) is 5.25g cm3。
Embodiment mode 11: the boride is titanium boride and the carbide is hafnium carbide
(1) Mixing titanium boride powder and hafnium carbide powder according to a mass ratio of 90:10, and carrying out ball milling by using a high-energy ball mill under the ball-material ratio of 40:1, the ball milling time of 20h and the rotating speed of 500r/min to obtain composite powder with uniform components and fine particles;
(2) placing the composite powder in a mould, and sintering in a discharge plasma furnace under the following conditions: and (3) heating the discharge plasma furnace to 2000 ℃ at the speed of 100 ℃/min, carrying out heat preservation sintering for 5min, wherein the sintering pressure is 50Mpa, and after sintering, cooling and demoulding to obtain the single-phase boride solid solution ceramic material (vvi).
The single-phase carborundum solid solution ceramic material (vvi) is characterized by mechanical properties, and the result shows that the hardness of the material at room temperature is 29 +/-4.2 GPa, the three-point bending strength is 477 +/-42 MPa, the elastic modulus is 425GPa, and the fracture toughness is 5.12 MPa.m1/2. And the density of the single-phase carborundum solid solution ceramic material (vvi) is 6.12g cm3。
Embodiment mode 12: the boride is titanium boride and the carbide is hafnium carbide
(1) Mixing titanium boride powder and hafnium carbide powder according to a mass ratio of 85:15, and carrying out ball milling by using a high-energy ball mill under the ball-material ratio of 40:1, the ball milling time of 30h and the rotating speed of 500r/min to obtain composite powder with uniform components and fine particles;
(2) placing the composite powder in a mould, and sintering in a hot pressing furnace under the following sintering conditions: and (2) heating the graphite heating body in the hot pressing furnace to 2100 ℃ at the speed of 20 ℃/min, carrying out heat preservation sintering for 1h at the sintering pressure of 50Mpa, and cooling and demoulding after sintering to obtain the single-phase carbon boride solid solution ceramic material (viii).
The single-phase carborundum solid solution ceramic material (viii) is characterized by mechanical properties, and the result shows that the hardness of the material at room temperature is 30 +/-1.3 GPa, the three-point bending strength is 477 +/-15 MPa, the elastic modulus is 410GPa, and the fracture toughness is 5.36 MPa.m1/2. And the density of the single-phase carborundum solid solution ceramic material (vvii) is 6.55g cm3。
Claims (5)
1. A preparation method of a single-phase carborundum solid solution ceramic material is characterized by comprising the following operation steps:
mixing boride-containing powder and carbide-containing powder, and performing high-energy ball milling to obtain composite powder;
the metal elements in the boron-containing compounds and the metal elements in the carbon-containing compounds are different metal elements;
the composite powder comprises 70-99% of boride-containing powder by mass and the balance of carbide-containing powder;
step two, placing the composite powder subjected to the high-energy ball milling in the step one in a mould for sintering to obtain a single-phase carborundum solid solution ceramic material;
the ball milling conditions of the high-energy ball mill in the first step are as follows: the ball-material ratio is 10-100: 1, the rotating speed is 400 r/min-800 r/min, and the ball milling time is 5-40 h;
sintering in the second step is plasma sintering or hot-pressing sintering;
the plasma sintering temperature is 1800-2300 ℃, and the sintering pressure is 30-80 MPa;
the hot-pressing sintering temperature is 1800-2300 ℃, and the sintering pressure is 30-80 MPa.
2. The method of preparing a single phase borocarbide solid solution ceramic material of claim 1, wherein: the boron-containing compound is titanium boride, zirconium boride, hafnium boride, niobium boride, tantalum boride, tungsten boride or molybdenum boride.
3. The method of preparing a single phase borocarbide solid solution ceramic material of claim 2, wherein: the carbide-containing substance is titanium carbide, zirconium carbide, hafnium carbide, niobium carbide, tantalum carbide, tungsten carbide or molybdenum carbide.
4. The method of preparing a single phase borocarbide solid solution ceramic material of claim 1, wherein: the plasma sintering is carried out in a discharge plasma furnace, and the sintering conditions are as follows: the sintering time is 5-60 min, and the heating rate is 50-150 ℃/min.
5. The method of preparing a single phase borocarbide solid solution ceramic material of claim 1, wherein: the sintering in the second step is carried out in a hot pressing furnace, and the sintering conditions are as follows: the sintering time is 0.5-10 h, and the heating rate is 10-40 ℃/min.
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