CN114605156B - TiB 2 Composite ceramic material for base armor - Google Patents
TiB 2 Composite ceramic material for base armor Download PDFInfo
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- CN114605156B CN114605156B CN202210254886.7A CN202210254886A CN114605156B CN 114605156 B CN114605156 B CN 114605156B CN 202210254886 A CN202210254886 A CN 202210254886A CN 114605156 B CN114605156 B CN 114605156B
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Abstract
The invention relates to a TiB 2 A base armor composite ceramic material belongs to the technical field of armor protection materials. The material is prepared from Ti powder, tiC powder and TiB 2 The powder is taken as a raw material, ball-milled, mixed and dried to obtain mixed powder, and then the mixed powder is subjected to discharge plasma sintering at a temperature T 1 Keeping the temperature and pressure at the pressure of 10 MPa-50 MPa, cooling, and then keeping the temperature at T 2 Is sintered, wherein T 1 ＝1200℃～1600℃，T 1 ―T 2 =100 ℃ to 150 ℃; cooling to obtain the composite ceramic material; ti powder, tiC powder and TiB 2 The sum of the powder mass is 100 percent, the mass fraction of Ti powder is 2 to 12 percent, the mass fraction of TiC powder is 10 to 30 percent, and the mass fraction of TiB powder is 2 The mass fraction of the powder is 58-88%. The composite ceramic material can be prepared at a lower sintering temperature, and has good hardness, strength and toughness.
Description
Technical Field
The invention relates to a TiB 2 A base armor composite ceramic material belongs to the technical field of armor protection materials.
Background
TiB 2 Because it is corrosion resistantHigh hardness, high modulus, high melting point, low density, and high strength at room temperature are considered ideal heavy armor protective materials that are commonly used in armor panels for combat vehicles to protect against penetration by large caliber armor-piercing projectiles and armor-breaking projectile jets.
However, tiB 2 Two major problems still exist with armor ceramic materials: poor toughness and high cost. This is because TiB 2 The preparation method has the characteristics of covalent bonding, high melting point and lower volume diffusion rate and grain boundary diffusion rate, when the preparation method is prepared by pressureless sintering or hot-pressing sintering and other methods, the prepared sintering temperature is up to 2000 ℃, so that the energy consumption is high, abnormal grain growth is easily caused in the preparation process, microcrack is caused in the cooling stage, and TiB is finally reduced 2 The mechanical properties of armor ceramic materials, especially the reduction of fracture toughness, greatly limits TiB 2 Armor ceramic materials are widely used.
In recent years, researchers at home and abroad find that the ceramic composite material has higher toughness and stronger multiple impact resistance of a bullet compared with simple substance ceramic. Therefore, researchers add multiple metallic, non-metallic secondary items to TiB 2 Improve the performance of the material. Wherein TiC has the characteristics of high melting point, good wear resistance and high hardness, and is mixed with TiB 2 Have good thermodynamic coexistence therebetween, and are considered to be excellent additive phases. However, in practice, tiC and TiB 2 All have the disadvantage of being difficult to densify. For this purpose, the conventional method is carried out by reacting Ti with B 4 C reaction, or TiO 2 And B 4 C reaction to produce TiB 2 -a TiC composite ceramic; however, the method has the advantages of long reaction time, large energy consumption, obvious coarsening of crystal grains and fixed proportion of products, and finally the mechanical property of the composite ceramic is poor. Alternatively, by directing the beam towards the TiB 2 Adding Ni, mo, fe and other TiB into TiC 2 Although the densification sintering temperature can be reduced to a certain degree by the method for promoting the densification of the ceramic by the high-density metal phase, the density of the composite ceramic is increased, the lightweight requirement of an armor protection material is not facilitated, and the relative performance of the newly generated brittleness material is adversely affected. Further, in general, tiB 2 Or a composite thereofThe densification sintering of the powder has higher requirement on the granularity of the powder, small-size micron powder or submicron powder is required to be prepared, and the preparation requirement is higher.
Disclosure of Invention
In view of the above, the present invention is to provide a TiB 2 The composite ceramic material is prepared from Ti powder, tiC powder and TiB 2 The powder is used as a raw material, and the TiB with good mechanical property is prepared by using a spark plasma sintering system at a lower sintering temperature 2 A composite ceramic material for base armor.
In order to achieve the purpose of the invention, the following technical scheme is provided.
TiB 2 The composite ceramic material of the base armor is prepared by Ti powder, tiC powder and TiB 2 The method comprises the steps of taking powder as a raw material, mixing the powder through ball milling, drying the powder to obtain mixed powder, sintering the mixed powder by using a spark plasma sintering system, and cooling the sintered powder to obtain the TiB 2 A base armor composite ceramic material;
ti powder, tiC powder and TiB 2 The sum of the powder mass is 100 percent, the mass fraction of Ti powder is 2 to 12 percent, the mass fraction of TiC powder is 10 to 30 percent, and the mass fraction of TiB powder is 2 The mass fraction of the powder is 58-88%;
the sintering treatment comprises the following steps: firstly, the sintering temperature is T 1 Keeping the temperature and the pressure for 1min to 2min under the condition that the sintering pressure is 10MPa to 50 MPa; then keeping the pressure unchanged, cooling, and waiting for the temperature to be reduced to T 2 Keeping the temperature and the pressure for 2-5 min; wherein T is 1 ＝1200℃～1600℃，T 1 ―T 2 ＝100℃～150℃。
Preferably, the average grain diameter of Ti powder is less than or equal to 60 mu m; the average grain size of TiC powder is less than or equal to 20 mu m; tiB 2 The average grain diameter of the powder is less than or equal to 15 mu m.
More preferably, the average particle size of Ti powder is less than or equal to 20 μm; the average grain diameter of the TiC powder is less than or equal to 2.6 mu m; tiB 2 The average grain diameter of the powder is less than or equal to 5 mu m.
Preferably, the ball milling medium of the ball milling is absolute ethyl alcohol; the ball-material ratio is (2-5) to 1; the ball milling speed is 150 r/min-350 r/min; the ball milling time is 2-4 h.
More preferably, the ball mill uses grinding balls composed of ZrO having a diameter of 15mm 2 ZrO of 10mm diameter ball 2 Balls and ZrO of 5mm diameter 2 The ball is composed of the following components in percentage by mass of 1.
Preferably, the drying process is as follows: and (3) carrying out vacuum drying on the mixed slurry obtained after the ball milling is finished at 70-85 ℃ for 0.5-1.5 h to completely volatilize the ball milling medium to obtain a mixed powder precursor, and drying the mixed powder precursor at 30-80 ℃ for 0.5-1 h to obtain the mixed powder.
More preferably, the vacuum drying is carried out by a vacuum rotary evaporator, and the rotating speed is 40 r/min-120 r/min.
Preferably, during the sintering process, the temperature of the spark plasma sintering system is raised to T 1 The specific method comprises the following steps: at a degree of vacuum<20Pa, the initial pressure is 1-4 MPa, the temperature is raised at the heating rate of 60-150 ℃/min, the pressure is increased when the temperature is raised to 900-1000 ℃, the temperature is raised at the heating rate of 30-50 ℃/min, and the temperature is raised to T when the temperature is raised to T 3 When the pressure reaches 10 MPa-50 MPa, the pressure is kept unchanged, and the temperature is continuously increased to T 1 (ii) a Wherein, T 1 ―T 3 =150 ℃ -200 ℃ and T 3 ＝1050℃～1400℃。
Preferably, the cooling after the completion of the sintering treatment is: keeping the pressure of the spark plasma sintering system unchanged, cooling at a cooling rate of 100 ℃/min, removing pressure when the temperature is reduced to be below 900 ℃, continuously cooling to be below 100 ℃ along with the furnace, and taking out the sintered ceramic block, wherein the ceramic block is TiB 2 The base armor composite ceramic material.
Advantageous effects
1. The invention provides a TiB 2 The base armor composite ceramic material comprises raw materials of Ti powder with the density of 4.51g/cm 3 The density of the TiC powder is 4.93g/cm 3 、TiB 2 The density of the powder was 4.52g/cm 3 The density of the three is very similar, the invention uses the method of spark plasma sintering to mix Ti powder, tiC powder and TiB powder with proper proportion and similar density 2 The powder is sintered, so that densification sintering can be realized at a lower temperature, and the strength and the toughness of the composite ceramic material are improved on the basis of ensuring good hardness. The addition of TiC ensures that the composite ceramic material has good hardness. On the basis, ti and TiB are generated in the sintering process 2 The generated TiB new phase is formed through a solid phase mechanism, and the TiB at the initial stage of sintering is filled 2 And the holes among the TiC particles, and part of incompletely reacted Ti is used as a liquid phase to fill the gaps, so that the high-density composite ceramic material can be obtained at a lower sintering temperature. TiC prevents TiB from growing continuously at high temperature and keeps the level of smaller grains; and sintering by means of the spark plasma sintering system has the characteristics of high heating rate and weak material transmission, can inhibit grain growth, obtain fine grains and improve the strength of the composite ceramic material. In addition, the grain boundary of the composite ceramic material increases a crack deflection path, and the toughness is improved. Among the reaction materials, ti and TiB 2 The TiB and a small amount of residual Ti after reaction can achieve the purposes of toughening and reinforcing through mechanisms such as plastic deformation, bridging and the like. Aiming at the problem, the invention can control TiC, tiB and TiB through controlling sintering conditions 2 The atoms in the phase are fully diffused and form a firm interface, and finer grains can be obtained to obtain better mechanical property.
2. The invention provides a TiB 2 The composite ceramic material of armor is prepared with micron level Ti powder, tiC powder and TiB powder of different grain sizes 2 The powder prepared composite ceramic material increases the mutual contact area between particles, reduces pores, increases sintering activity and weakens the TiB pair by combining the collocation of coarse particles and fine particles on the basis of the collocation of raw materials 2 Requirement of powder size, i.e. not requiring small size TiB 2 Micron powder or TiB 2 Submicron powder can obtain the densified composite ceramic material. In addition, coarsening of crystal grains is inhibited through interaction among different particles, and the strength of the material is improved.
3. The invention provides a TiB 2 The base armor composite ceramic material adopts a ball milling mode to mix reaction raw materialsMore uniform, zrO of 2 Hard balls, zrO during ball milling 2 The ball cannot be abraded; and the grinding balls with different sizes can fully and uniformly mix the raw material powder, which is beneficial to obtaining the composite ceramic with uniform organization structure subsequently.
4. The invention provides a TiB 2 The base armor composite ceramic material raises the temperature of the spark plasma sintering system to T 1 In the temperature rise process, the temperature rise is carried out at the temperature rise rate of 60-150 ℃/min, and the reason is that if the temperature rise rate is too high, the activation time of particles is short, the air in pores is not exhausted in time, and the density is greatly reduced; if the temperature rise rate is too slow, the sintering cycle will be lengthened, the crystal grains will be coarsened, and the material properties will be impaired. The temperature is increased at the heating rate of 30-50 ℃/min, which aims to reduce the thermal stress gradient in the die and the material, avoid the fracture of the TiB phase which is unstable in thermodynamics and mechanics in the pressurizing process under the temperature and stress gradient to generate internal microscopic defects and reduce the performance of the composite ceramic. Finally, the invention firstly heats up to T 3 Then heating to T 1 The aim is to promote the close contact among particles, reduce the pores and accelerate the densification process in the middle and later periods of temperature rise.
5. The invention provides a TiB 2 After the sintering treatment is finished, the base armor composite ceramic material is cooled at the cooling rate of 100 ℃/min, so that the influence of residual stress generated in the cooling process on the structure and the performance of the composite ceramic material can be inhibited
Drawings
FIG. 1 is an SEM image of fine grain morphology at fracture for example 2.
FIG. 2 is an SEM image of TiB morphology of the polished surface of example 2.
Detailed Description
The invention is further illustrated by the following detailed description, wherein the processes are conventional unless otherwise specified, and the starting materials are commercially available or may be prepared from literature.
The following examples:
the Ti powder is produced by Beijing Xinglong source technology Co., ltd, and has an average particle size of 20 μm and a purity of 99.5%.
The TiC powder is produced by Beijing Xinglong source technology Limited, and has the average grain diameter of 2.6 mu m and the purity of 99.8 percent.
The TiB 2 The powder was produced by Dengdong Nichin technologies, inc. and had an average particle size of 5 μm and a purity of 99.8%.
The absolute ethyl alcohol is produced by Guangdong fine chemical company in Beijing.
The actual density was measured and calculated according to the method specified in the national standard GB/T25995-2010 Fine ceramic Density and apparent porosity test method.
The calculation formula of the density D is as follows: d = ρ Practice of /ρ Theory of the invention X 100%, where ρ In fact Representing the actual density, p Theory of the invention Indicating the theoretical density.
The vickers hardness was measured by using an HV-1000A micro vickers hardness tester manufactured by the laboratory pilot incorporated of the garden east china.
The three-point bending strength is tested according to the method specified in the national standard GB/T6569-2006 Fine ceramic bending Strength test method.
The fracture toughness is tested according to a method specified in the national standard GB/T23806-2009 Fine ceramic fracture toughness test method unilateral pre-crack Beam (SEPB) method.
Example 1
(1) 9.6g of Ti powder, 36g of TiC powder and 74.4g of TiB 2 Adding the powder into a ball milling tank of a planetary ball mill, and adding grinding balls and excessive absolute ethyl alcohol according to the ball-to-material ratio of 3 2 ZrO of 10mm diameter ball 2 Balls and ZrO of 5mm diameter 2 The ball is composed according to the mass ratio of 1: 2; ball milling for 2 hours at the rotating speed of 200r/min, and uniformly mixing to obtain mixed slurry; pouring the mixed slurry into a vacuum rotary evaporator, and carrying out rotary evaporation for 0.5h under the conditions that the rotating speed is 80r/min and the water bath temperature is 85 ℃ to completely volatilize the ball-milling medium, thus obtaining a mixed powder precursor; placing the mixed powder precursor into an electric heating constant temperature blast drying oven, and drying at 60 deg.CDrying for 1h to obtain mixed powder.
(2) Putting 120g of the mixed powder into a graphite mould with the inner diameter of 60mm, separating the mixed powder from the graphite mould by graphite paper with the thickness of 0.1mm, wrapping the outer layer of the graphite mould by using a stone felt, putting the graphite mould into a discharge plasma sintering system, and setting the initial vacuum degree in a furnace cavity<20Pa, initial pressure of 4MPa, heating at 60 deg.C/min, increasing pressure when temperature rises to 900 deg.C, heating at 30 deg.C/min, and heating to T 3 =1050 ℃, when the pressure reaches 40MPa, the pressure is kept unchanged, and the temperature is continuously increased to T 1 Keeping the temperature and the pressure for 1min when the temperature is not higher than 1200 ℃, then keeping the pressure unchanged, cooling, and cooling to T 2 Keeping the temperature and the pressure for 3min when the temperature is not less than 1100 ℃; then keeping the pressure unchanged, and cooling at the cooling rate of 100 ℃/min; when the temperature is reduced to 900 ℃, the pressure is removed, the furnace is continuously cooled to 100 ℃, and the sintered ceramic block is taken out, namely the TiB 2 A base armor composite ceramic material; and then removing graphite paper adhered to the surface of the ceramic block body, cleaning the surface of the ceramic block body by using deionized water, cleaning the surface of the ceramic block body by using ethanol, naturally drying, and carrying out subsequent tests.
Cleaning and drying TiB 2 The base armor composite ceramic material was tested as follows:
(1) Observing the micro morphology of the composite ceramic material by using a scanning electron microscope (SEM, hitachi S-4800), wherein a sintered sample presents a fine-grained structure according to a fracture fine-grained morphology SEM picture; according to the polished surface TiB morphology SEM picture, the sintered sample has TiB rod crystals; the two microstructure structures are beneficial to improving the strength and the toughness of the composite ceramic.
(2) Calculating the density through the actual density and the theoretical density of the composite ceramic material: the TiB 2 The actual density of the base armor composite ceramic material is 4.60g/cm 3 Theoretical density of 4.63g/cm 3 The density is 99.3%.
(3) The Vickers hardness, the three-point bending strength and the fracture toughness of the composite ceramic material are tested, and the test results are as follows: dimension under load of 9.8NThe hardness value is 22.3GPa; the three-point bending strength is 733MPa; the fracture toughness is 7.71 MPa.m 1 /2 。
Example 2
(1) 2.4g of Ti powder, 9g of TiC powder and 18.6g of TiB 2 Adding the powder into a ball milling tank of a planetary ball mill, and adding grinding balls and excessive absolute ethyl alcohol according to the ball-to-material ratio of 3 2 ZrO of 10mm diameter ball or sphere 2 Balls and ZrO of 5mm diameter 2 The ball is composed of the following components in a mass ratio of 1; ball-milling for 2 hours at the rotating speed of 200r/min, and uniformly mixing to obtain mixed slurry; pouring the mixed slurry into a vacuum rotary evaporator, and carrying out rotary evaporation for 0.5h under the conditions that the rotating speed is 80r/min and the water bath temperature is 85 ℃ to completely volatilize the ball-milling medium, thus obtaining a mixed powder precursor; and (3) putting the mixed powder precursor into an electric heating constant-temperature air blast drying box, and drying at 60 ℃ for 1 hour to obtain mixed powder.
(2) Placing 30g of the mixed powder into a graphite mold with an inner diameter of 20mm, separating the mixed powder from the graphite mold by graphite paper with a thickness of 0.1mm, wrapping the graphite mold with a stone felt on the outer layer, placing the graphite mold into a discharge plasma sintering system, and setting the initial vacuum degree in a furnace cavity<20Pa, initial pressure of 4MPa, heating at 60 deg.C/min, increasing pressure when temperature rises to 900 deg.C, heating at 30 deg.C/min, and heating to T 3 =1250 ℃ and the pressure reaches 40MPa, the pressure is kept unchanged, and the temperature is continuously increased to T 1 Keeping the temperature and the pressure for 1min when the temperature is not less than 1450 ℃, then keeping the pressure unchanged, cooling, and cooling to T 2 Keeping the temperature and the pressure for 3min when the temperature is not larger than 1300 ℃; then keeping the pressure unchanged, cooling at the cooling rate of 100 ℃/min, removing the pressure when the temperature is reduced to 900 ℃, continuously cooling to 100 ℃ along with the furnace, taking out the sintered ceramic block, namely the TiB 2 A base armor composite ceramic material; and then removing graphite paper adhered to the surface of the ceramic block body, cleaning the surface of the ceramic block body by using deionized water, cleaning the surface of the ceramic block body by using ethanol, naturally drying, and carrying out subsequent tests.
Cleaning and drying TiB 2 Composite ceramic for base armorThe materials were tested as follows:
(1) The microscopic morphology of the composite ceramic material is observed by a scanning electron microscope (SEM, hitachi S-4800), the test results are shown in figures 1 and 2, and as can be seen from figure 1, a sintered sample has a fine crystalline structure; as can be seen from fig. 2, tiB rod crystals were present in the sintered sample. The two microstructure structures are beneficial to improving the strength and the toughness of the composite ceramic.
(2) Calculating the density through the actual density and the theoretical density of the composite ceramic material: the TiB 2 The actual density of the base armor composite ceramic material is 4.61g/cm 3 Theoretical density of 4.63g/cm 3 The density is 99.6%.
(3) The Vickers hardness, the three-point bending strength and the fracture toughness of the composite ceramic material are tested, and the test results are as follows: the Vickers hardness value under a load of 9.8N is 22.6GPa; the three-point bending strength is 848MPa; the fracture toughness is 7.78 MPa.m 1 /2 . Combining the performance test data of the composite ceramic material prepared in example 1, it can be seen that in examples 1 and 2, ti powder, tiC powder and TiB powder 2 The relative amounts of the powders were the same except that the composite ceramic material prepared in example 1 was larger in size than that of example 2. As is known in the art, the larger the size of the composite ceramic, the lower the mechanical properties. However, the mechanical properties of hardness, strength and toughness of the composite ceramic materials prepared in examples 1 and 2 are still maintained at a good level, which indicates that the composite ceramic materials prepared by the preparation method of the present invention can obtain good mechanical properties even if the composite ceramic materials are large in size.
Example 3
(1) 3.6g of Ti powder, 9g of TiC powder and 17.4g of TiB 2 Adding the powder into a ball milling tank of a planetary ball mill, and adding grinding balls and excessive absolute ethyl alcohol according to the ball-to-material ratio of 3 2 ZrO of 10mm diameter ball or sphere 2 Balls and ZrO of 5mm diameter 2 The ball comprises the following components in percentage by mass; ball milling for 2 hours at the rotating speed of 200r/min, and uniformly mixing to obtain mixed slurry; pouring the mixed slurry into a vacuum rotary evaporatorPerforming rotary evaporation for 0.5h under the conditions that the rotating speed is 80r/min and the water bath temperature is 85 ℃ to completely volatilize the ball milling medium, thereby obtaining a mixed powder precursor; and (3) putting the mixed powder precursor into an electric heating constant-temperature air-blast drying oven, and drying at 60 ℃ for 1h to obtain mixed powder.
(2) Placing 30g of the mixed powder into a graphite mold with an inner diameter of 20mm, separating the mixed powder from the graphite mold by graphite paper with a thickness of 0.1mm, wrapping the graphite mold with a stone felt on the outer layer, placing the graphite mold into a discharge plasma sintering system, and setting the initial vacuum degree in a furnace cavity<20Pa, initial pressure of 4MPa, heating at a heating rate of 90 deg.C/min, increasing pressure when temperature rises to 900 deg.C, heating at a heating rate of 40 deg.C/min, and heating to T 3 Keeping the pressure unchanged at 1320 ℃ and 10MPa, and continuously heating to T 1 Keeping the temperature and the pressure for 1min when the temperature is not less than 1520 ℃, then keeping the pressure unchanged, cooling, and cooling to T 2 Keeping the temperature and the pressure for 3min when the temperature is not less than 1400 ℃; then keeping the pressure unchanged, cooling at the cooling rate of 100 ℃/min, removing the pressure when the temperature is reduced to 900 ℃, continuing to cool to 100 ℃ along with the furnace, and taking out the sintered ceramic block, namely the TiB 2 A base armor composite ceramic material; and then removing graphite paper adhered to the surface of the ceramic block body, cleaning the surface of the ceramic block body by using deionized water, cleaning the surface of the ceramic block body by using ethanol, naturally drying, and carrying out subsequent tests.
The TiB after being cleaned and dried is treated 2 The base armor composite ceramic material was tested as follows:
(1) Observing the micro morphology of the composite ceramic material by using a scanning electron microscope (SEM, hitachi S-4800), wherein a sintered sample presents a fine-grained structure according to a fracture fine-grained morphology SEM picture; according to the SEM image of the TiB morphology of the polished surface, tiB rod crystals exist in the sintered sample; the two microstructure structures are beneficial to improving the strength and the toughness of the composite ceramic.
(2) Calculating the density through the actual density and the theoretical density of the composite ceramic material: the TiB 2 The actual density of the base armor composite ceramic material is 4.59g/cm 3 Has a theoretical density of 4.63 g-cm 3 The density is 99.1%.
(3) The Vickers hardness, the three-point bending strength and the fracture toughness of the composite ceramic material are tested, and the test result is as follows: the Vickers hardness value under a load of 9.8N is 21.0GPa; the three-point bending strength is 660MPa; the fracture toughness is 6.35 MPa.m 1 /2 。
Example 4
(1) 1.2g of Ti powder, 6g of TiC powder and 22.8g of TiB 2 Adding the powder into a ball milling tank of a planetary ball mill, and adding grinding balls and excessive absolute ethyl alcohol according to the ball-material ratio of 3 2 ZrO of 10mm diameter ball 2 Balls and ZrO of 5mm diameter 2 The ball comprises the following components in percentage by mass; ball-milling for 2 hours at the rotating speed of 200r/min, and uniformly mixing to obtain mixed slurry; pouring the mixed slurry into a vacuum rotary evaporator, and carrying out rotary evaporation for 0.5h under the conditions that the rotating speed is 80r/min and the water bath temperature is 85 ℃ to completely volatilize the ball-milling medium, thus obtaining a mixed powder precursor; and (3) putting the mixed powder precursor into an electric heating constant-temperature air-blast drying oven, and drying at 60 ℃ for 1h to obtain mixed powder.
(2) Placing 30g of the mixed powder into a graphite mold with an inner diameter of 20mm, separating the mixed powder from the graphite mold by graphite paper with a thickness of 0.1mm, wrapping the graphite mold with a stone felt on the outer layer, placing the graphite mold into a discharge plasma sintering system, and setting the initial vacuum degree in a furnace cavity<Heating at the initial pressure of 4MPa and the heating rate of 150 ℃/min under 20Pa, increasing the pressure when the temperature is increased to 1000 ℃, and heating at the heating rate of 50 ℃/min; when the temperature rises to T 3 Keeping the pressure unchanged at 1300 ℃ and 50MPa, and continuously heating to T 1 Keeping the temperature and the pressure for 2min when the temperature is not less than 1500 ℃, keeping the pressure unchanged, cooling, and cooling to T 2 Keeping the temperature and the pressure for 3min when the temperature is not larger than 1350 ℃; then keeping the pressure unchanged, cooling at the cooling rate of 100 ℃/min, removing the pressure when the temperature is reduced to 900 ℃, continuing to cool to 100 ℃ along with the furnace, and taking out the sintered ceramic block, namely the TiB 2 A base armor composite ceramic material; then removing the graphite paper adhered on the surface of the ceramic block body, and firstly using deionized waterAnd (3) cleaning the surface of the ceramic block by water, cleaning the surface of the ceramic block by ethanol, naturally drying, and carrying out subsequent tests.
Cleaning and drying TiB 2 The base armor composite ceramic material was tested as follows:
(1) Observing the microstructure of the composite ceramic material by using a scanning electron microscope (SEM, hitachi S-4800), wherein a sintered sample presents a fine-grained structure according to a fracture fine-grained morphology SEM picture; according to the polished surface TiB morphology SEM picture, the sintered sample has TiB rod crystals; the two microstructure structures are beneficial to improving the strength and the toughness of the composite ceramic.
(2) Calculating the density through the actual density and the theoretical density of the composite ceramic material: the TiB 2 The actual density of the base armor composite ceramic material is 4.55g/cm 3 Theoretical density of 4.6g/cm 3 The compactness is 99.0%.
(3) The Vickers hardness, the three-point bending strength and the fracture toughness of the composite ceramic material are tested, and the test results are as follows: the Vickers hardness value under a load of 9.8N is 23.1GPa; the three-point bending strength is 677MPa; the fracture toughness is 7.21 MPa.m 1 /2 。
Example 5
(1) 0.6g of Ti powder, 3g of TiC powder and 26.4g of TiB 2 Adding the powder into a ball milling tank of a planetary ball mill, and adding grinding balls and excessive absolute ethyl alcohol according to the ball-material ratio of 3 2 ZrO of 10mm diameter ball 2 Balls and ZrO of 5mm diameter 2 The ball is composed of the following components in a mass ratio of 1; ball-milling for 2 hours at the rotating speed of 200r/min, and uniformly mixing to obtain mixed slurry; pouring the mixed slurry into a vacuum rotary evaporator, and carrying out rotary evaporation for 0.5h under the conditions that the rotating speed is 80r/min and the water bath temperature is 85 ℃ to completely volatilize the ball-milling medium, thus obtaining a mixed powder precursor; and (3) putting the mixed powder precursor into an electric heating constant-temperature air-blast drying oven, and drying at 60 ℃ for 1h to obtain mixed powder.
(2) 30g of the mixed powder was put into a graphite mold having an inner diameter of 20mm, and 0 was used between the mixed powder and the graphite mold.Separating graphite paper with thickness of 1mm, wrapping graphite mold with graphite felt, placing into discharge plasma sintering system, and setting initial vacuum degree in furnace cavity<20Pa, initial pressure of 4MPa, heating at a rate of 150 deg.C/min, increasing pressure when the temperature is up to 980 deg.C, heating at a rate of 50 deg.C/min, and heating to T 3 Keeping the pressure unchanged when the temperature is 1400 ℃ and the pressure reaches 40MPa, and continuously heating to T 1 Keeping the temperature and the pressure for 2min when the temperature is more than 1600 ℃, then keeping the pressure unchanged, cooling, and cooling to T 2 Keeping the temperature and the pressure for 2min when the temperature is not less than 1450 ℃; then keeping the pressure unchanged, cooling at the cooling rate of 100 ℃/min, removing the pressure when the temperature is reduced to 900 ℃, continuously cooling to 100 ℃ along with the furnace, taking out the sintered ceramic block, namely the TiB 2 A base armor composite ceramic material; and then removing graphite paper adhered to the surface of the ceramic block body, cleaning the surface of the ceramic block body by using deionized water, cleaning the surface of the ceramic block body by using ethanol, naturally drying, and carrying out subsequent tests.
The TiB after being cleaned and dried is treated 2 The base armor composite ceramic material was tested as follows:
(1) Observing the micro morphology of the composite ceramic material by using a scanning electron microscope (SEM, hitachi S-4800), wherein a sintered sample presents a fine-grained structure according to a fracture fine-grained morphology SEM picture; according to the polished surface TiB morphology SEM picture, the sintered sample has TiB rod crystals; the two microstructure structures are beneficial to improving the strength and the toughness of the composite ceramic.
(2) Calculating the density through the actual density and the theoretical density of the composite ceramic material: the TiB 2 The actual density of the base armor composite ceramic material is 4.52g/cm 3 Theoretical density of 4.56g/cm 3 The density is 99.2%.
(3) The Vickers hardness, the three-point bending strength and the fracture toughness of the composite ceramic material are tested, and the test results are as follows: the Vickers hardness value under the load of 9.8N is 22.7GPa; the three-point bending strength is 606MPa; the fracture toughness is 6.80 MPa.m 1 /2 。
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 should be considered as being within the scope of the present invention.
Claims (9)
1. TiB 2 The base armor composite ceramic material is characterized in that: the material is prepared from Ti powder, tiC powder and TiB 2 The method comprises the following steps of taking powder as a raw material, mixing the powder through ball milling, drying the powder to obtain mixed powder, sintering the mixed powder by using a spark plasma sintering system, and cooling to obtain the TiB 2 A base armor composite ceramic material;
ti powder, tiC powder and TiB 2 The sum of the powder mass is 100%, the mass fraction of Ti powder is 2-12%, the mass fraction of TiC powder is 10-30%, and TiB 2 The mass fraction of the powder is 58-88%;
the sintering treatment comprises the following steps: firstly, the sintering temperature is T 1 Keeping the temperature and the pressure for 1min to 2min under the condition that the sintering pressure is 10MPa to 50 MPa; then keeping the pressure unchanged, cooling, and waiting for the temperature to be reduced to T 2 Keeping the temperature and the pressure for 2-5 min; wherein T is 1 ＝1200℃～1600℃，T 1 ―T 2 ＝100℃～150℃；
Raising the temperature of the spark plasma sintering system to T 1 The specific method comprises the following steps: at a degree of vacuum<20Pa, initial pressure of 1-4 MPa, heating at a rate of 60-150 deg.C/min, increasing pressure when the temperature rises to 900-1000 deg.C, heating at a rate of 30-50 deg.C/min, and heating to T 3 When the pressure reaches 10 MPa-50 MPa, the pressure is kept unchanged, and the temperature is continuously increased to T 1 (ii) a Wherein, T 1 ―T 3 =150 ℃ -200 ℃ and T 3 ＝1050℃～1400℃。
2. A TiB according to claim 1 2 The base armor composite ceramic material is characterized in that: the average grain diameter of Ti powder is less than or equal to 60 mu m; the average grain size of TiC powder is less than or equal to 20 mu m; tiB 2 The average grain diameter of the powder is less than or equal to 15 mu m.
3. A TiB according to claim 2 2 The base armor composite ceramic material is characterized in that: the average grain diameter of Ti powder is less than or equal to 20 mu m; the average grain diameter of the TiC powder is less than or equal to 2.6 mu m; tiB 2 The average grain diameter of the powder is less than or equal to 5 mu m.
4. A TiB according to claim 1 2 The base armor composite ceramic material is characterized in that: the ball milling medium of the ball milling is absolute ethyl alcohol; the ball-material ratio is (2-5) to 1; the ball milling speed is 150 r/min-350 r/min; the ball milling time is 2-4 h.
5. A TiB according to claim 4 2 The base armor composite ceramic material is characterized in that: the grinding ball used in the ball milling is made of ZrO with the diameter of 15mm 2 ZrO of 10mm diameter ball or sphere 2 Balls and ZrO of 5mm diameter 2 The ball is composed of the following components in percentage by mass of 1.
6. A TiB according to claim 1 2 The base armor composite ceramic material is characterized in that: the drying process comprises the following steps: and (3) carrying out vacuum drying on the mixed slurry obtained after the ball milling is finished at 70-85 ℃ for 0.5-1.5 h to completely volatilize the ball milling medium to obtain a mixed powder precursor, and drying the mixed powder precursor at 30-80 ℃ for 0.5-1 h to obtain the mixed powder.
7. A TiB according to claim 6 2 The base armor composite ceramic material is characterized in that: the vacuum drying is carried out by adopting a vacuum rotary evaporator, and the rotating speed is 40 r/min-120 r/min.
8. A TiB according to any one of claims 1 to 7 2 The base armor composite ceramic material is characterized in that: the cooling after the sintering treatment is as follows: keeping the pressure of the spark plasma sintering system unchanged, cooling at a cooling rate of 100 ℃/min, discharging the pressure when the temperature is reduced to below 900 ℃, continuously cooling to below 100 ℃ along with the furnace, and taking out the sintered ceramicBlock body, i.e. a TiB 2 The base armor composite ceramic material.
9. A TiB according to claim 3 2 The base armor composite ceramic material is characterized in that: the ball milling medium of the ball milling is absolute ethyl alcohol; the ball material ratio is (2-5) to 1; the ball milling speed is 150 r/min-350 r/min; the ball milling time is 2-4 h;
the grinding ball used in the ball milling is made of ZrO with the diameter of 15mm 2 ZrO of 10mm diameter ball 2 Balls and ZrO of 5mm diameter 2 The ball is composed of the following components in a mass ratio of 1;
the drying process comprises the following steps: vacuum drying the mixed slurry obtained after the ball milling is finished at 70-85 ℃ for 0.5-1.5 h to ensure that the ball milling medium is completely volatilized to obtain a mixed powder precursor, and drying the mixed powder precursor at 30-80 ℃ for 0.5-1 h to obtain the mixed powder;
the vacuum drying is carried out by adopting a vacuum rotary evaporator, and the rotating speed is 40 r/min-120 r/min;
the cooling after the sintering treatment is as follows: keeping the pressure of the spark plasma sintering system unchanged, cooling at a cooling rate of 100 ℃/min, discharging the pressure when the temperature is reduced to be below 900 ℃, continuously cooling to be below 100 ℃ along with the furnace, and taking out the sintered ceramic block, namely the TiB 2 A composite ceramic material for base armor.
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