原位合成CeB_6/B_4C陶瓷材料的力学性能和显微组织研究
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摘要
碳化硼是一种重要的特种陶瓷,具有高硬度、低密度、高熔点、良好的中子吸收能力和抗化学侵蚀能力等优良性能,但是韧性较差限制了其更广泛的应用。本论文以提高碳化硼材料的韧性为目标,首次采用原位合成和热压烧结相结合的方法制备了CeB6/B4C陶瓷材料,分别对纯B4C陶瓷材料、热压烧结CeB6/B4C陶瓷材料和原位合成CeB6/B4C陶瓷材料的力学性能和显微组织进行了研究；并对CeO2-B4C-C反应体系的热力学和动力学进行了分析。在此基础上,进一步研究了原位合成CeB6/B4C陶瓷材料的界面微结构、原位反应热压烧结机理和增韧补强机制。研究结果表明：
在2040℃×20MPa×40min优化条件下热压烧结制备的纯B4C陶瓷材料的体积密度为2.419g/cm3,维氏硬度为31.34 GPa,抗弯强度为268.76 MPa,断裂韧性为3.14MPa·m1/2。随着温度的升高,纯B4C陶瓷材料的气孔率先降低后略有增大；保温时间对纯B4C陶瓷材料的气孔率影响不明显,但其晶粒随着保温时间的增加而变大,尤其在高温下保温时间太长,晶粒会急剧长大。
在1950℃×20MPa×40min的优化条件下制备的热压烧结CeB6/B4C陶瓷材料的相对密度为96.95%,维氏硬度为39.97GPa,抗弯强度为313.81 Mpa,断裂韧性为4.55 MPa-m1/2,相对于纯B4C材料分别提高了0.96%、27.53%、16.76%和44.90%。第二相CeB6的添加,降低了碳化硼陶瓷材料的烧结温度。热压烧结CeB6/B4C陶瓷材料的气孔率大幅度降低,没有出现明显的晶粒长大现象。
在1950℃×20MPa×40min的条件下制备的原位合成CeB6/B4C陶瓷材料的相对密度为97.92%,维氏硬度为42.01GPa,抗弯强度为346.75 Mpa,断裂韧性为5.95 MPa-m1/2,相对于热压烧结CeB6/B4C陶瓷材料分别提高了1.01%、5.10%、10.50%和30.77%,相对于纯B4C材料分别提高了2.01%、34.04%、29.02%和89.49%。Ce02和B4C原位生成CeB6的化学反应导致Ce02和B4C两相之间产生约5 nm的非晶过渡层,使相界面结合良好,对其界面结合强度起到了增强作用。原位生成的CeB6对晶界活动性产生很大的影响,其具有抑制晶粒长大的作用,故CeB6弥散分布在组织中,在晶粒细化方面大有裨益。细晶增韧补强、第二相颗粒和基体之间的热膨胀系数不匹配产生的残余应力导致的裂纹偏转、第二相拔出和沿晶断裂是原位合成CeB6/B4C陶瓷材料的主要增韧补强机制。
CeO2、B4C和C的高温化学反应属于CeO2-B4C-C多组元化学反应体系。TG-DTA和XRD的实验结果表明,CeO2、B4C和C反应生成CeB6经历了5个步骤：①650～910℃时,CeO2和B4C反应生成CeBO3、CeBC和B,表观活化能E1为271.5kJ·mol-1,反应级数n1为0.24;②1270～1309℃时,Ce02和B4C反应生成CeBO3、B、CeB4和CO,CeBC、CeBO3和B4C反应生成CeB4和CO,其表观活化能E2为241.9kJ·mol-1,反应级数n2为0.16；③1317～1370℃时,CeBO3、B4C和C反应生成CeB4、B和CO,其表观活化能E3为715.1kJ·mol-1,反应级数n3为0.41；④1371～1420℃时,CeO2、B4C和C反应生成CeB4和CO；⑤1460℃时,CeB4和B反应生成CeB6,表观活化能E4为327.1kJ·mol-1,反应级数n4为0.13。1460℃时,随着时间延长,CeB6量增加,CeB4和单质B量减少,2h时,CeB6量达到了97.8%,CeB4基本上已全部转化为CeB6。1460℃以上的温度,CeO2、B4C和C反应原位合成CeB6/B4C陶瓷材料是可行的。
Boron carbide is a kind of important special ceramics, which has excellent properties, such as high hardness, low density, high melting point, and high capability for neutron absorption, as well as good resistance to chemical corrosion. However, the shortage of boron carbide material is its extreme susceptibility to brittle fracture, which limit its application. In order to improve its fracture toughness, CeB6/B4C ceramic material were prepared by in-situ synthesis and hot pressed sintering method. The mechanical properties and microstructure of pure B4C ceramic material, hot pressed sintering CeB6/B4C ceramic material and in-situ synthesis CeB6/B4C ceramic material were studied respectively, and the thermodynamics and kinetics of CeO2-B4C-C system were researched, the interface microstructure, and in-situ reaction hot pressed sintering mechanism, as well as toughening and reinforcing mechanisms of in-situ synthesis CeB6/B4C ceramics were also investigated. The studied results indicated that:
In the case of 2040℃×20MPa×40min, the density of pure B4C ceramic material is 2.419g/cm3, the Vickers-microhardness 31.34 GPa, the bending strength 268.76 MPa, the fracture toughness 3.14 MPa·m1/2. With the temperature increasing, its porosity decreases first, then increases. The effect of sintering time on the porosity of pure B4C ceramic material isn't obvious. However, its crystal grain grows with sintering time, and especially grows more fast when sintering time is much longer at high temperature.
In the case of 1950℃×20MPa×40min, the relative density of hot pressed sintering CeB6/B4C ceramic material is 96.95%, the Vickers-microhardness 39.97 GPa, the bending strength 313.81 MPa, the fracture toughness 4.55 MPa-m1/2, which enhance 0.96%, 27.53%,16.76% and 44.90% respectively compared to that of pure B4C ceramic material. The sintering temperature of boron carbide ceramics is decreased by adding second-phase CeB6. The porosity of hot pressed sintering CeB6/B4C ceramic material decreases and there is no crystal grain growth.
In the case of 1950℃×20MPa×40min, the relative density of in-situ synthesis ceramic material is 97.92%, the Vickers-microhardness 42.01 GPa, the bending strength 346.75 MPa, the fracture toughness 5.95 MPa·m1/2 which improve 1.01%, 5.10%,10.50% and 30.77% respectively compared to that of hot pressed sintering CeB6/B4C ceramic material, and improve 2.01%,34.04%,29.02% and 89.49% respectively compared to that of pure B4C ceramic material. A amorphous transition layer of 5nm-width CeB6, synthesized in-situ by CeO2 and B4C, make the interface combine very well, and intensify the combination strength of interfaces. The in-situ synthesized CeB6 greatly impact grain boundary mobility, and inhibits grain growth. Therefore, in-situ synthesized CeB6 disperse among the structure, and play good role at grain refinement. The main toughening and reinforcing mechanisms of in-situ synthesis CeB6/B4C ceramic material were:fine grain toughening and reinforcing, the crack deflection caused by the residual stress resulting from the difference in thermal expansion coefficient between CeB6 and B4C, the second-phase CeB6 pullout and intergranular crack.
The chemical reaction among CeO2, B4C and C under high temperature belongs to CeO2-B4C-C multicomponent chemical reaction system. The TG-DTA and XRD experimental results illustrates the process of CeO2, B4C and C generating CeB6 undergo five steps, firstly, at 650～910℃, CeO2, B4C and C react into CeBO3, CeBC and B, and the apparent activation energy (E1) is 271.5kJ·mol-1, the series (n1) is 0.24; secondly, at 1270～1309℃, CeO2 and B4C react into CeBO3, B and CeB4, at the same time, CeBO3, CeBC and B4C react into CeB4, and the apparent activation energy (E2) is 241.9kJ·mol-1, the series(n2) is 0.16; thirdly, at 1317～1370℃, CeBO3, B4C and C react into CeB4 and B, and the apparent activation energy (E3) is 715.1kJ·mol, the series(n3) is 0.41; fourthly, in 1371～1420℃, CeO2, B4C and C react into CeB6 and CO; fifthly, at the temperature of 1460℃,CeB4 and B further react into CeB6, and the apparent activation energy (E4) is 327.1 kJ·mol-1, the series(m4) is 0.13. With the prolonging time, the content of CeB6 increases but the content of CeB4 and B decrease, the content of CeB6 is 97.8% at 2 h, and most CeB4 changes into CeB6. It is feasible that in-situ synthesis CeB6/B4C ceramic material by the reaction of CeO2, B4C and C above 1460℃.
在2040℃×20MPa×40min优化条件下热压烧结制备的纯B4C陶瓷材料的体积密度为2.419g/cm3,维氏硬度为31.34 GPa,抗弯强度为268.76 MPa,断裂韧性为3.14MPa·m1/2。随着温度的升高,纯B4C陶瓷材料的气孔率先降低后略有增大；保温时间对纯B4C陶瓷材料的气孔率影响不明显,但其晶粒随着保温时间的增加而变大,尤其在高温下保温时间太长,晶粒会急剧长大。
在1950℃×20MPa×40min的优化条件下制备的热压烧结CeB6/B4C陶瓷材料的相对密度为96.95%,维氏硬度为39.97GPa,抗弯强度为313.81 Mpa,断裂韧性为4.55 MPa-m1/2,相对于纯B4C材料分别提高了0.96%、27.53%、16.76%和44.90%。第二相CeB6的添加,降低了碳化硼陶瓷材料的烧结温度。热压烧结CeB6/B4C陶瓷材料的气孔率大幅度降低,没有出现明显的晶粒长大现象。
在1950℃×20MPa×40min的条件下制备的原位合成CeB6/B4C陶瓷材料的相对密度为97.92%,维氏硬度为42.01GPa,抗弯强度为346.75 Mpa,断裂韧性为5.95 MPa-m1/2,相对于热压烧结CeB6/B4C陶瓷材料分别提高了1.01%、5.10%、10.50%和30.77%,相对于纯B4C材料分别提高了2.01%、34.04%、29.02%和89.49%。Ce02和B4C原位生成CeB6的化学反应导致Ce02和B4C两相之间产生约5 nm的非晶过渡层,使相界面结合良好,对其界面结合强度起到了增强作用。原位生成的CeB6对晶界活动性产生很大的影响,其具有抑制晶粒长大的作用,故CeB6弥散分布在组织中,在晶粒细化方面大有裨益。细晶增韧补强、第二相颗粒和基体之间的热膨胀系数不匹配产生的残余应力导致的裂纹偏转、第二相拔出和沿晶断裂是原位合成CeB6/B4C陶瓷材料的主要增韧补强机制。
CeO2、B4C和C的高温化学反应属于CeO2-B4C-C多组元化学反应体系。TG-DTA和XRD的实验结果表明,CeO2、B4C和C反应生成CeB6经历了5个步骤：①650～910℃时,CeO2和B4C反应生成CeBO3、CeBC和B,表观活化能E1为271.5kJ·mol-1,反应级数n1为0.24;②1270～1309℃时,Ce02和B4C反应生成CeBO3、B、CeB4和CO,CeBC、CeBO3和B4C反应生成CeB4和CO,其表观活化能E2为241.9kJ·mol-1,反应级数n2为0.16；③1317～1370℃时,CeBO3、B4C和C反应生成CeB4、B和CO,其表观活化能E3为715.1kJ·mol-1,反应级数n3为0.41；④1371～1420℃时,CeO2、B4C和C反应生成CeB4和CO；⑤1460℃时,CeB4和B反应生成CeB6,表观活化能E4为327.1kJ·mol-1,反应级数n4为0.13。1460℃时,随着时间延长,CeB6量增加,CeB4和单质B量减少,2h时,CeB6量达到了97.8%,CeB4基本上已全部转化为CeB6。1460℃以上的温度,CeO2、B4C和C反应原位合成CeB6/B4C陶瓷材料是可行的。
Boron carbide is a kind of important special ceramics, which has excellent properties, such as high hardness, low density, high melting point, and high capability for neutron absorption, as well as good resistance to chemical corrosion. However, the shortage of boron carbide material is its extreme susceptibility to brittle fracture, which limit its application. In order to improve its fracture toughness, CeB6/B4C ceramic material were prepared by in-situ synthesis and hot pressed sintering method. The mechanical properties and microstructure of pure B4C ceramic material, hot pressed sintering CeB6/B4C ceramic material and in-situ synthesis CeB6/B4C ceramic material were studied respectively, and the thermodynamics and kinetics of CeO2-B4C-C system were researched, the interface microstructure, and in-situ reaction hot pressed sintering mechanism, as well as toughening and reinforcing mechanisms of in-situ synthesis CeB6/B4C ceramics were also investigated. The studied results indicated that:
In the case of 2040℃×20MPa×40min, the density of pure B4C ceramic material is 2.419g/cm3, the Vickers-microhardness 31.34 GPa, the bending strength 268.76 MPa, the fracture toughness 3.14 MPa·m1/2. With the temperature increasing, its porosity decreases first, then increases. The effect of sintering time on the porosity of pure B4C ceramic material isn't obvious. However, its crystal grain grows with sintering time, and especially grows more fast when sintering time is much longer at high temperature.
In the case of 1950℃×20MPa×40min, the relative density of hot pressed sintering CeB6/B4C ceramic material is 96.95%, the Vickers-microhardness 39.97 GPa, the bending strength 313.81 MPa, the fracture toughness 4.55 MPa-m1/2, which enhance 0.96%, 27.53%,16.76% and 44.90% respectively compared to that of pure B4C ceramic material. The sintering temperature of boron carbide ceramics is decreased by adding second-phase CeB6. The porosity of hot pressed sintering CeB6/B4C ceramic material decreases and there is no crystal grain growth.
In the case of 1950℃×20MPa×40min, the relative density of in-situ synthesis ceramic material is 97.92%, the Vickers-microhardness 42.01 GPa, the bending strength 346.75 MPa, the fracture toughness 5.95 MPa·m1/2 which improve 1.01%, 5.10%,10.50% and 30.77% respectively compared to that of hot pressed sintering CeB6/B4C ceramic material, and improve 2.01%,34.04%,29.02% and 89.49% respectively compared to that of pure B4C ceramic material. A amorphous transition layer of 5nm-width CeB6, synthesized in-situ by CeO2 and B4C, make the interface combine very well, and intensify the combination strength of interfaces. The in-situ synthesized CeB6 greatly impact grain boundary mobility, and inhibits grain growth. Therefore, in-situ synthesized CeB6 disperse among the structure, and play good role at grain refinement. The main toughening and reinforcing mechanisms of in-situ synthesis CeB6/B4C ceramic material were:fine grain toughening and reinforcing, the crack deflection caused by the residual stress resulting from the difference in thermal expansion coefficient between CeB6 and B4C, the second-phase CeB6 pullout and intergranular crack.
The chemical reaction among CeO2, B4C and C under high temperature belongs to CeO2-B4C-C multicomponent chemical reaction system. The TG-DTA and XRD experimental results illustrates the process of CeO2, B4C and C generating CeB6 undergo five steps, firstly, at 650～910℃, CeO2, B4C and C react into CeBO3, CeBC and B, and the apparent activation energy (E1) is 271.5kJ·mol-1, the series (n1) is 0.24; secondly, at 1270～1309℃, CeO2 and B4C react into CeBO3, B and CeB4, at the same time, CeBO3, CeBC and B4C react into CeB4, and the apparent activation energy (E2) is 241.9kJ·mol-1, the series(n2) is 0.16; thirdly, at 1317～1370℃, CeBO3, B4C and C react into CeB4 and B, and the apparent activation energy (E3) is 715.1kJ·mol, the series(n3) is 0.41; fourthly, in 1371～1420℃, CeO2, B4C and C react into CeB6 and CO; fifthly, at the temperature of 1460℃,CeB4 and B further react into CeB6, and the apparent activation energy (E4) is 327.1 kJ·mol-1, the series(m4) is 0.13. With the prolonging time, the content of CeB6 increases but the content of CeB4 and B decrease, the content of CeB6 is 97.8% at 2 h, and most CeB4 changes into CeB6. It is feasible that in-situ synthesis CeB6/B4C ceramic material by the reaction of CeO2, B4C and C above 1460℃.
引文
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