CN107200586B - TiB2Rapid preparation method of ceramic block - Google Patents
TiB2Rapid preparation method of ceramic block Download PDFInfo
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- CN107200586B CN107200586B CN201710535947.6A CN201710535947A CN107200586B CN 107200586 B CN107200586 B CN 107200586B CN 201710535947 A CN201710535947 A CN 201710535947A CN 107200586 B CN107200586 B CN 107200586B
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Abstract
The invention relates to a TiB2A rapid preparation method of a ceramic block belongs to the field of functional protection material preparation. The method is carried out by mixing TiB2Adding the powder and Al powder into a ball milling tank, uniformly mixing, and drying to obtain mixed powder; sintering the mixed powder by adopting a spark plasma sintering system to obtain the TiB2A ceramic block. The electric field can clean and activate the particle surfaces of the mixed powder in the sintering process, so that the densification process of the mixed powder is carried out at a lower sintering temperature, the sintering time is greatly shortened, and TiB obtained by sintering is2The ceramic block has high density, high hardness and good comprehensive performance, and can be applied to the field of protective materials; the method is simple and easy to implement, short in period and strong in practicability, and is beneficial to industrialization.
Description
Technical Field
The invention relates to a TiB2A rapid preparation method of a ceramic block belongs to the field of functional protection material preparation.
Background
TiB2The lattice structure of the ceramic material is a close-packed hexagonal structure, and the lattice structure is combined with each other by covalent bonds, is an extremely stable superhard ceramic material, and has excellent physical and chemical propertiesChemical and mechanical properties, such as: high melting point (2980 ℃), high hardness (34GPa), corrosion resistance, good high-temperature performance, high electrical conductivity, high thermal conductivity (20 W.m.K-25 W.m.K) and relatively low density (4.5 g/cm)3) The application range of the method is extremely wide, almost relates to various departments of national economy and various fields of modern technology, and plays an important role in promoting the development of industry and the improvement of productivity.
At present, TiB is prepared2The ceramic block mainly comprises pressureless sintering, hot-pressing sintering, self-propagating high-temperature synthesis and the like. But TiB2The Ti-B ionic bond and the B-B covalent bond between the surface of the boron atom and the surface of the titanium atom determine that the sintering performance of the material is poor, and the conventional sintering method needs high sintering temperature and long sintering time. Previous researches show that TiB with the density of more than 95 percent is difficult to obtain by a pressureless sintering process2A ceramic block. While the ceramic block with higher density can be obtained by hot-pressing sintering and self-propagating high-temperature synthesis, the sintering temperature is high (not less than 1800 ℃) and the time is long (not less than 1 h). For example, researchers in the national laboratory of Oak Ridge in the United states adopt a hot pressing process to keep the temperature at 1800 ℃ for 2 hours to obtain TiB with the relative density of more than 97 percent2A material.
In addition, the coarsening of the crystal grains caused by the long time consumption of the traditional sintering can also cause the TiB2The strength of the ceramic block is reduced. Sullggi and Baik et al, the foreign scholars, showed that TiB increases with grain size2Residual stress in the ceramic increases rapidly, resulting in a large amount of microcracking and deterioration of mechanical properties. How to obtain fully compact TiB while avoiding abnormal grain growth2The ceramic sintered body is a problem of concern to the present researchers.
Disclosure of Invention
In view of the above, the present invention is to provide a TiB2The rapid preparation method of the ceramic block adopts a spark plasma sintering system, and realizes TiB by adding a small amount of Al powder (0.5 wt% -5 wt%) which is used as a sintering aid and a gap filler in the sintering process2The ceramic block is prepared quickly, controllably and at low cost. The method provided by the invention can reduce the sintering temperature (less than or equal to)1750 ℃), greatly shortens the sintering time (less than or equal to 30min), improves the compactness and improves the mechanical property of the material, and is an ideal choice for the ceramic material in the future composite protective material.
The purpose of the invention is realized by the following technical scheme.
TiB2The rapid preparation method of the ceramic block comprises the following steps:
(1) mixing TiB2Adding the powder and Al powder into a ball milling tank, uniformly mixing to obtain mixed slurry, and drying to obtain mixed powder;
wherein, TiB2The mass ratio of the powder to the Al powder is (19-199): 1;
TiB is preferred2The particle size of the powder is less than or equal to 20 mu m; the grain size of the preferred Al powder is less than or equal to 80 mu m;
preferably, the ball milling adopts an SM-QB planetary ball mill;
the preferred ball milling parameters are: the ball milling medium is absolute ethyl alcohol; the ball material ratio is 3: 1; the rotating speed of the ball mill is 300r/min, and the ball milling time is 0.5 h-1 h;
the grinding balls are preferably composed of large agate balls and small agate balls in a mass ratio of 1:1, the diameter of each large agate ball is 10mm, and the diameter of each small agate ball is 5 mm;
preferably, the drying process is as follows:
firstly, carrying out vacuum drying on the mixed slurry after ball milling at 70-80 ℃, and drying at 30-80 ℃ for 0.5-1 h after the ball milling medium is volatilized;
preferably, the vacuum drying adopts a vacuum rotary evaporator, and the rotating speed of the vacuum rotary evaporator is 40 r/min-100 r/min;
(2) sintering the mixed powder by adopting a spark plasma sintering system to obtain the TiB of the invention2A ceramic block.
Wherein, the sintering process is as follows:
heating at a heating rate of 60-180 ℃/min under the conditions that the initial vacuum degree is less than 15Pa and the initial pressure is 0.2-1 MPa; when the temperature is raised to 600 ℃, the temperature raising rate is adjusted to be below 30 ℃/min; when the temperature is higher than 680 ℃ and the displacement rate variation of the sintered mixed powder is less than or equal to 0.02mm/s, adjusting the temperature rise rate to be 50-120 ℃/min; when the temperature is higher than 1200-1700 ℃ and the vacuum degree is less than 15Pa, adjusting the heating rate to 30-50 ℃/min, pressurizing simultaneously, and keeping the temperature and pressure for 3-15 min after the temperature is raised to 1250-1750 ℃ and the pressure reaches 5-50 MPa; then keeping the pressure unchanged, cooling to below 900 ℃ along with the furnace, removing the pressure, and cooling to below 100 ℃ along with the furnace.
Advantageous effects
1. The invention provides a TiB2The rapid preparation method of the ceramic block adopts TiB2The mixed powder of powder and Al powder is used as raw material, a spark plasma sintering system is adopted for sintering, the electric field can clean and activate the particle surfaces of the mixed powder in the sintering process, the densification process of the mixed powder is carried out at a lower sintering temperature (1250-1750 ℃), the sintering time is greatly shortened (less than or equal to 30min), and TiB obtained by sintering2The ceramic block has high density (the density can reach 99.7 percent), high hardness (the density can reach 32.8GPa) and good comprehensive performance, and can be applied to the field of protective materials;
2. the invention provides a TiB2The rapid preparation method of the ceramic block is simple and easy to implement, short in period, strong in practicability and beneficial to industrialization.
Drawings
FIG. 1 shows TiB prepared in examples 1 to 42Thickness and density values of the ceramic block.
FIG. 2 shows TiB prepared in examples 1 to 42Vickers hardness values of ceramic blocks.
Detailed Description
The invention is described in detail below with reference to the figures and the specific embodiments.
TiB described in the examples below2The powder was produced by Dengdong Nichin technologies, Inc. and had an average particle size of 3 μm and a purity of 99.8%.
The Al powder is produced by the Henan ocean aluminum industry Co Ltd, the average grain diameter is 20 μm, and the purity is 99.5%; the components and mass fractions (wt%) thereof are shown in table 2:
TABLE 2
The absolute ethyl alcohol is produced by Guangdong fine chemical company in Beijing.
The vickers hardness was measured using a L M700AT microhardness tester manufactured by L ECO.
The actual density was determined according to the method specified in the national Standard GB/T1423-1996 test methods for the Density of noble metals and alloys thereof.
The calculation formula of the density D is as follows: d ═ ρPractice of/ρTheory of the invention× 100%, where ρPractice ofRepresenting the actual density, pTheory of the inventionRepresenting the theoretical density.
Example 1
TiB2The rapid preparation method of the ceramic block comprises the following steps:
(1) 99.5g of TiB2Adding the powder and 0.5g of Al powder into a ball milling tank of an SM-QB planetary ball mill, and adding grinding balls and excessive absolute ethyl alcohol according to a ball-to-material ratio of 3: 1; ball-milling for 0.5h at the rotating speed of 300r/min, and uniformly mixing to obtain mixed slurry; pouring the mixed slurry into a vacuum rotary evaporator, and steaming for 0.5h under the conditions that the rotating speed is 100r/min and the water bath temperature is 80 ℃ to obtain a mixed powder precursor; and (3) putting the mixed powder precursor into an electric heating constant-temperature air drying oven, and drying for 1h at the temperature of 60 ℃ to obtain mixed powder.
The grinding ball is composed of a large agate ball and a small agate ball in a mass ratio of 1:1, the diameter of the large agate ball is 10mm, and the diameter of the small agate ball is 5 mm.
(2) Placing 100g of mixed powder into a graphite mold with an inner diameter of 60mm, wrapping the graphite mold with asbestos felt, placing into a spark plasma sintering system, and setting an initial vacuum degree in a furnace cavity<15Pa, the initial pressure is 0.2MPa, the temperature is raised at the heating rate of 60 ℃/min, and when the temperature is raised to 600 ℃, the heating rate is adjusted to be 30 ℃/min; when the temperature is higher than 680 ℃ and the displacement rate variation of the sintered mixed powder is less than or equal to 0.02mm/s, adjusting the temperature rise rate to be 50 ℃/min; when the temperature is higher than1700 ℃ and degree of vacuum<Adjusting the heating rate to 30 ℃/min when the pressure is 15Pa, simultaneously pressurizing, keeping the temperature and the pressure for 15min when the temperature is increased to 1750 ℃ and the pressure reaches 5 MPa; then keeping the pressure unchanged, cooling to below 900 ℃ along with the furnace, removing the pressure, cooling to below 100 ℃ along with the furnace, taking out the sintered ceramic block, and cleaning the surface of the ceramic by using ethanol and deionized water to obtain the TiB2A ceramic block.
As shown in FIG. 1, TiB2The thickness of the ceramic block body is 7.96mm, and the density is 98.9%; as shown in FIG. 2, for the TiB2The Vickers hardness of the ceramic block was measured and maintained at a test force of 300gf for 10 seconds, and the Vickers hardness value was found to be 32.8 GPa.
Example 2
TiB2The rapid preparation method of the ceramic block comprises the following steps:
(1) 95g of TiB2Adding the powder and 5g of Al powder into a ball milling tank of an SM-QB planetary ball mill, and adding grinding balls and excessive absolute ethyl alcohol according to a ball-to-material ratio of 3: 1; ball-milling for 1h at the rotating speed of 300r/min, and uniformly mixing to obtain mixed slurry; pouring the mixed slurry into a vacuum rotary evaporator, and steaming for 0.5h under the conditions that the rotating speed is 40r/min and the water bath temperature is 80 ℃ to obtain a mixed powder precursor; and (3) putting the mixed powder precursor into an electric heating constant-temperature air drying oven, and drying at 30 ℃ for 0.5h to obtain mixed powder.
The grinding ball is composed of a large agate ball and a small agate ball in a mass ratio of 1:1, the diameter of the large agate ball is 10mm, and the diameter of the small agate ball is 5 mm.
(2) Placing 100g of mixed powder into a graphite mold with an inner diameter of 60mm, wrapping the graphite mold with asbestos felt, placing into a spark plasma sintering system, and setting an initial vacuum degree in a furnace cavity<15Pa, the initial pressure is 1MPa, the temperature is raised at the rate of 180 ℃/min, and when the temperature is raised to 600 ℃, the temperature raising rate is adjusted to be 20 ℃/min; when the temperature is higher than 680 ℃ and the displacement rate variation of the sintered mixed powder is less than or equal to 0.02mm/s, adjusting the temperature rise rate to be 120 ℃/min; when the temperature is higher than 1200 ℃ and the vacuum degree is high<Adjusting the heating rate to 50 ℃/min when the pressure is 15Pa, pressurizing simultaneously,keeping the temperature and pressure for 3min when the temperature is 1250 ℃ and the pressure reaches 50 MPa; then keeping the pressure unchanged, cooling to below 900 ℃ along with the furnace, removing the pressure, cooling to below 100 ℃ along with the furnace, taking out the sintered ceramic block, and cleaning the surface of the ceramic by using ethanol and deionized water to obtain the TiB2A ceramic block.
As shown in FIG. 1, TiB2The thickness of the ceramic block body is 8.13mm, and the density is 99.7%; as shown in FIG. 2, for the TiB2The Vickers hardness of the ceramic block was measured and maintained at a test force of 300gf for 10 seconds, and the Vickers hardness value was found to be 31.3 GPa.
Example 3
TiB2The rapid preparation method of the ceramic block comprises the following steps:
(1) 398g of TiB2Adding the powder and 2g of Al powder into a ball milling tank of an SM-QB planetary ball mill, and adding grinding balls and excessive absolute ethyl alcohol according to a ball-to-material ratio of 3: 1; ball-milling for 0.5h at the rotating speed of 300r/min, and uniformly mixing to obtain mixed slurry; pouring the mixed slurry into a vacuum rotary evaporator, and steaming for 0.5h under the conditions that the rotating speed is 100r/min and the water bath temperature is 80 ℃ to obtain a mixed powder precursor; and (3) putting the mixed powder precursor into an electric heating constant-temperature air drying oven, and drying for 1h at the temperature of 60 ℃ to obtain mixed powder.
The grinding ball is composed of a large agate ball and a small agate ball in a mass ratio of 1:1, the diameter of the large agate ball is 10mm, and the diameter of the small agate ball is 5 mm.
(2) Placing 400g of mixed powder into a graphite mold with an inner diameter of 60mm, wrapping the graphite mold with asbestos felt, placing the graphite mold into a spark plasma sintering system, and setting an initial vacuum degree in a furnace cavity<15Pa, the initial pressure is 0.2MPa, the temperature is raised at the heating rate of 60 ℃/min, and when the temperature is raised to 600 ℃, the heating rate is adjusted to be 30 ℃/min; when the temperature is higher than 680 ℃ and the displacement rate variation of the sintered mixed powder is less than or equal to 0.02mm/s, adjusting the temperature rise rate to be 50 ℃/min; when the temperature is higher than 1700 ℃ and the vacuum degree is high<Adjusting the heating rate to 30 ℃/min when the pressure is 15Pa, simultaneously pressurizing, keeping the temperature and the pressure for 15min when the temperature is increased to 1750 ℃ and the pressure reaches 5 MPa; then firstly keeping the pressureCooling to below 900 deg.c, releasing pressure, cooling to below 100 deg.c, taking out sintered ceramic block, and washing the surface of the ceramic block with alcohol and deionized water to obtain TiB2A ceramic block.
As shown in FIG. 1, TiB2The thickness of the ceramic block is 32.03mm, and the density is 98.3%; as shown in FIG. 2, for the TiB2The Vickers hardness of the ceramic block was measured and maintained at a test force of 300gf for 10 seconds, and the Vickers hardness value was found to be 31.1 GPa.
Example 4
TiB2The rapid preparation method of the ceramic block comprises the following steps:
(1) 380g of TiB2Adding the powder and 20g of Al powder into a ball milling tank of an SM-QB planetary ball mill, and adding grinding balls and excessive absolute ethyl alcohol according to a ball-to-material ratio of 3: 1; ball-milling for 1h at the rotating speed of 300r/min, and uniformly mixing to obtain mixed slurry; pouring the mixed slurry into a vacuum rotary evaporator, and steaming for 0.5h under the conditions that the rotating speed is 40r/min and the water bath temperature is 80 ℃ to obtain a mixed powder precursor; and (3) putting the mixed powder precursor into an electric heating constant-temperature air drying oven, and drying at 30 ℃ for 0.5h to obtain mixed powder.
The grinding ball is composed of a large agate ball and a small agate ball in a mass ratio of 1:1, the diameter of the large agate ball is 10mm, and the diameter of the small agate ball is 5 mm.
(2) Placing 400g of mixed powder into a graphite mold with an inner diameter of 60mm, wrapping the graphite mold with asbestos felt, placing the graphite mold into a spark plasma sintering system, and setting an initial vacuum degree in a furnace cavity<15Pa, the initial pressure is 1MPa, the temperature is raised at the rate of 180 ℃/min, and when the temperature is raised to 600 ℃, the temperature raising rate is adjusted to be 20 ℃/min; when the temperature is higher than 680 ℃ and the displacement rate variation of the sintered mixed powder is less than or equal to 0.02mm/s, adjusting the temperature rise rate to be 120 ℃/min; when the temperature is higher than 1200 ℃ and the vacuum degree is high<Adjusting the heating rate to 50 ℃/min when the pressure is 15Pa, simultaneously pressurizing, keeping the temperature and the pressure for 3min when the temperature is increased to 1250 ℃ and the pressure reaches 50 MPa; then keeping the pressure unchanged, cooling to below 900 ℃ along with the furnace, removing the pressure, cooling to below 100 ℃ along with the furnace, and taking outCleaning the surface of the sintered ceramic block by using ethanol and deionized water to obtain TiB2A ceramic block.
As shown in FIG. 1, TiB2The thickness of the ceramic block body is 32.93mm, and the density is 98.5%; as shown in FIG. 2, for the TiB2The Vickers hardness of the ceramic block was measured and maintained at a test force of 300gf for 10 seconds, and the Vickers hardness value was 30.4 GPa.
The present invention includes, but is not limited to, the above embodiments, and any equivalent substitutions or partial modifications made under the principle of the spirit of the present invention are considered to be within the scope of the present invention.
Claims (10)
1. TiB2The rapid preparation method of the ceramic block is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing TiB2Adding the powder and Al powder into a ball milling tank, uniformly mixing to obtain mixed slurry, and drying to obtain mixed powder;
TiB2the mass ratio of the powder to the Al powder is (19-199): 1;
(2) sintering the mixed powder by adopting a spark plasma sintering system to obtain the TiB2A ceramic block;
the sintering process is as follows:
heating at a heating rate of 60-180 ℃/min under the conditions that the initial vacuum degree is less than 15Pa and the initial pressure is 0.2-1 MPa; when the temperature is raised to 600 ℃, the temperature raising rate is adjusted to be below 30 ℃/min; when the temperature is higher than 680 ℃ and the displacement rate variation of the sintered mixed powder is less than or equal to 0.02mm/s, adjusting the temperature rise rate to be 50-120 ℃/min; when the temperature is higher than 1200-1700 ℃ and the vacuum degree is less than 15Pa, adjusting the heating rate to 30-50 ℃/min, pressurizing simultaneously, and keeping the temperature and pressure for 3-15 min after the temperature is raised to 1250-1750 ℃ and the pressure reaches 5-50 MPa; then keeping the pressure unchanged, cooling to below 900 ℃ along with the furnace, removing the pressure, and cooling to below 100 ℃ along with the furnace.
2. A TiB according to claim 12Ceramic blockA method for rapidly preparing a body, which is characterized in that: TiB2The particle size of the powder is less than or equal to 20 mu m; the grain diameter of the Al powder is less than or equal to 80 mu m.
3. A TiB according to claim 1 or 22The rapid preparation method of the ceramic block is characterized by comprising the following steps: the ball milling adopts an SM-QB planetary ball mill.
4. A TiB according to claim 1 or 22The rapid preparation method of the ceramic block is characterized by comprising the following steps: the ball milling parameters are as follows: the ball milling medium is absolute ethyl alcohol; the ball material ratio is 3: 1; the rotating speed of the ball mill is 300r/min, and the ball milling time is 0.5 h-1 h.
5. A TiB according to claim 42The rapid preparation method of the ceramic block is characterized by comprising the following steps: the grinding ball is composed of a large agate ball and a small agate ball in a mass ratio of 1:1, the diameter of the large agate ball is 10mm, and the diameter of the small agate ball is 5 mm.
6. A TiB according to claim 1 or 22The rapid preparation method of the ceramic block is characterized by comprising the following steps: the drying process comprises the following steps: and (3) carrying out vacuum drying on the mixed slurry after ball milling at 70-80 ℃, and drying at 30-80 ℃ for 0.5-1 h after the ball milling medium is volatilized.
7. A TiB according to claim 62The rapid preparation method of the ceramic block is characterized by comprising the following steps: the ball milling parameters are as follows: the vacuum drying adopts a vacuum rotary evaporator, and the rotating speed is 40 r/min-100 r/min.
8. A TiB according to claim 1 or 22The rapid preparation method of the ceramic block is characterized by comprising the following steps: the ball milling adopts an SM-QB planetary ball mill;
the ball milling parameters are as follows: the ball milling medium is absolute ethyl alcohol; the ball material ratio is 3: 1; the rotating speed of the ball mill is 300r/min, and the ball milling time is 0.5 h-1 h;
the grinding ball is composed of a large agate ball and a small agate ball in a mass ratio of 1:1, the diameter of the large agate ball is 10mm, and the diameter of the small agate ball is 5 mm.
9. A TiB according to claim 82The rapid preparation method of the ceramic block is characterized by comprising the following steps: and (3) carrying out vacuum drying on the mixed slurry after ball milling at 70-80 ℃, and drying at 30-80 ℃ for 0.5-1 h after the ball milling medium is volatilized.
10. A TiB according to claim 92The rapid preparation method of the ceramic block is characterized by comprising the following steps: the ball milling parameters are as follows: the vacuum drying adopts a vacuum rotary evaporator, and the rotating speed is 40 r/min-100 r/min.
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| CN201710535947.6A CN107200586B (en) | 2017-07-04 | 2017-07-04 | TiB2Rapid preparation method of ceramic block |
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| CN102610531A (en) * | 2012-03-12 | 2012-07-25 | 华中科技大学 | Method for preparing diamond-silicon composite package material |
| CN103553631B (en) * | 2013-10-24 | 2015-03-25 | 中国科学院金属研究所 | Method for obtaining compact titanium diboride material by using in-situ reaction between sintering aids |
| CN106396688A (en) * | 2016-09-14 | 2017-02-15 | 北京理工大学 | Fast preparation method of TiB-TiC-TiB2-B4C composite ceramic |
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| CN102610531A (en) * | 2012-03-12 | 2012-07-25 | 华中科技大学 | Method for preparing diamond-silicon composite package material |
| CN103553631B (en) * | 2013-10-24 | 2015-03-25 | 中国科学院金属研究所 | Method for obtaining compact titanium diboride material by using in-situ reaction between sintering aids |
| CN106396688A (en) * | 2016-09-14 | 2017-02-15 | 北京理工大学 | Fast preparation method of TiB-TiC-TiB2-B4C composite ceramic |
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