Nb、Al合金化MoSi_2的合成、组织与性能研究
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摘要
MoSi_2及其硅化物基材料被认为是一种非常有潜力的可用于1200℃以上的高温结构材料，但存在室温断裂韧性差、高温易蠕变以及低温粉化瘟疫的缺陷。针对上述问题，本文以Nb单一合金化和Nb、Al协同合金化MoSi_2为思路，利用固体与分子经验电子理论进行材料理论设计与性能预测，通过热力学计算了理论绝热燃烧温度，采用燃烧合成技术获得超过饱和固溶体，运用真空热压烧结和放电等离子烧结技术使其致密化，并对其组织和性能进行研究。
根据固体与分子经验电子理论，对C11_b型MeS_2（Me=Mo,Nb；S=Si,Al）价电子结构的计算表明，Nb、Al合金化引起C11_b相中原子杂化状态变化，使C11_b相中最强键及次强键的键能及键上共价电子对数的下降，导致宏观硬度降低；Nb单一合金化提高了C11_b相中共价电子数比例值，有利于提高C11_b相的强度；Al单一合金化和微量Nb、Al协同合金化均使值下降，导致C11_b相强度下降。
采用双亚点阵模型对(Mo_(1-x)Nb_x)Si_2和Mo(Si_(1-y)Al_y)_2体系的理论绝热温度进行了模拟计算，结果表明Nb或Al的固溶引起C11_b相和C40相热容及热焓的变化，从而改变体系的绝热温度，实验设计成分(Mo_(1-x)Nb_x)Si_2和Mo(Si_(1-y)Al_y)_2的理论绝热温度均高于1800K，可以在室温下由元素粉末通过燃烧合成反应生成。
以Mo、Si、Nb、Al元素粉末为原料，通过燃烧合成技术制备了(Mo_(1-x)Nb_x)Si_2、Mo (Si_(1-y)Al_y)2和(Mo_(1-x)Nb_x)(Si_(1-y)Al_y)_2合金。燃烧合成产物主要为固溶有Nb(Al)的C11_b相和C40相，存在过饱和固溶现象。Nb合金化促进NbSi_2及MoSi_2型C40相形成，Al单一合金化及Nb、Al协同合金化促进Mo(Si,Al)_2型C40相的形成。Nb、Al合金化促进了MoSi_2燃烧合成反应的放热，使燃烧温度上升，其反应机制为：熔融-溶解-析出。
以燃烧合成产物为原料，分别采用真空热压烧结和放电等离子烧结制备了致密的(Mo_(1-x)Nb_x)Si_2和(Mo_(1-x)Nb_x)(Si_(1-y)Al_y)_2合金，C11_b相中过饱和固溶的Nb/Al在烧结过程中发生脱溶形成C40相。热压使合金相组成趋近于平衡状态。放电等离子烧结速度快、温度低，形成的合金晶粒细小且仍存在过饱和C11_b相。
系统研究了热压合金的室温力学性能，结果表明：少量Nb固溶使(Mo_(1-x)Nb_x)Si_2合金室温硬度下降，弯曲强度升高，对断裂韧性无显著影响。大量Nb使C40相增加，导致硬度上升，强度和断裂韧性下降。Nb和Al协同合金化对室温弯曲强度的影响不大，有Nb存在时，Al添加量达一定值（y=0.15）会显著恶化MoSi_2的强度。少量Nb和Al协同合金化可显著提高室温断裂韧性，最高达到10.7MPa/m~(1/2)，比纯MoSi_2提高了74%，增加合金量促使形成Mo(Si,Al)2型C40相导致(Mo_(1-x)Nb_x)(Si_(1-y)Al_y)_2合金断裂韧性降低而硬度升高。
对放电等离子烧结合金的室温和高温力学性能进行了系统研究，结果表明：放电等离子烧结合金的强度和硬度均高于同成分热压合金。放电等离子烧结(Mo_(1-x)Nb_x)Si_2合金的强度、硬度和断裂韧性变化趋势和热压合金一致，但断裂韧性下降较慢。Nb的增加使(Mo_(1-x)Nb_x)Si_2合金高温压缩强度呈现出先增后降的趋势，(Mo_(0.85)Nb_(0.15))Si_2合金的高温强度达到246MPa，比MoSi_2提高了110%。(Mo_(0.85)Nb_(0.15))Si_2合金高温变形经历了整体变形和玻璃相集中变形两个阶段，玻璃相集中变形使高温流变应力下降，而MoSi_2只经历了整体变形阶段。Nb、Al协同合金化可更有效的改善高温性能，Nb在高温下起到固溶强化作用，并且有助于产生层错强化效应；少量Al可减少晶界SiO2玻璃相使高温强度上升，但大量Al合金化会降低C11_b和C40相的高温强度；(Mo_(0.85)Nb_(0.15)(Si_(0.97)Al_(0.03))_2合金在1400℃具有最高的压缩强度，达到252MPa，该合金同时还具有最佳室温综合力学性能。
热压工艺制备的合金在500℃没有发生粉化瘟疫现象。Nb单一合金化加剧了MoSi_2的低温氧化，通过高温预氧化处理可在(Mo_(1-x)Nb_x)Si_2表面形成保护性氧化膜，提高低温抗氧化性能。Nb和Al协同合金化MoSi_2的低温抗氧化性优于Nb单一合金化，Nb的作用仍然是加速低温氧化，而Al则有利于抑制低温氧化。(Mo_(0.97)Nb_(0.03)(Si_(0.97)Al_(0.03))_2合金低温氧化性能优于纯MoSi_2。大量合金元素不利于高温预氧化保护膜的形成，大量Al促进氧化形成没有自愈合作用的莫来石-氧化铝复合氧化膜，大量Nb促使MoO_3形成，MoO_3在高温下气化，导致氧化膜出现大量孔洞，不能产生保护作用，甚至恶化材料的低温抗氧化性能。
Nb,Al alloyed MoSi_2was synthesized by combustion synthesis in this work. Thecombustion mode, combustion temperature, reaction mechanism, flame-frontpropagation velocity and product structure were investigated. Then dense materialwas prepared by vacuum hot pressing sintering and sparks plasma sintering usingcombustion synthesis products as raw materials. The organizations and propertieswere studied, and the action mechanisms of alloys were clarified.
From the element powders,(Mo_(1-x)Nb_x)Si_2, Mo(Si_(1-y)Al_y)_2and(Mo_(1-x)Nb_x)(Si_(1-y)Al_y)_2alloys were successfully synthesized by the mode ofself-propagating high-temperature synthesis. And the combustion products are formedthrough melting, dissolution and precipitation mechanism in combustion synthesis. Simelts first in alloys without Al, while Al-Si eutectic melt firstly forms after whichSi-rich melt forms in alloys containing Al. Solid Nb and Mo dissolute into the meltwhen contacted with it, and then reaction products precipitate from the supersaturatedsolution.
Using combustion synthesis products as raw materials, dense (Mo_(1-x)Nb_x)Si_2and(Mo_(1-x)Nb_x)(Si_(1-y)Al_y)_2alloy were prepared by vacuum hot pressing sintering and sparkplasma sintering. The precipitation reaction occurs during the sintering process andC40phase forms by Nb/Al precipitate from supersaturated C11_b phase. The phasecomposition of HP alloy is close to the equilibrium state, while saturated C11_bphasecould also be found in the SPS alloys together with tiny grains, because thetemperature is low and time is short in spark plasma sintering process.
For HP alloys, a little Nb solid solution raises the bending strength from216Mpato284MPa, a small amount of Nb and Al co-alloying could significantly increase thefracture toughness at room temperature, up to10.7MPa/m~(1/2), which is74%higherthan pure MoSi_2; but massive alloys promote the formation of C40phase and result inthe decreasing of fracture toughness and increasing of hardness. For SPS alloys,(Mo0.85Nb0.15)(Si_(0.97)Al_(0.03))_2alloy shows the best combination of high-temperaturecompression strength and best room-temperature mechanical properties, and itsstrength at1400℃is252MPa, which is115%higher than pure MoSi_2.
No pesting phenomena were observed in HP alloys when oxidized at at500℃.Nb alloying accelerates the low-temperature oxidation of MoSi_2, while Al isadvantageous for inhibiting oxidation at500℃.(Mo_(0.97)Nb_(0.03)(Si_(0.97)Al_(0.03))_2shows thebest oxidation performance in all alloys. An approach for avoiding low-temperature oxidation was put forward. A glass protective scale can be formed on the surface of(Mo_(1-x)Nb_x)Si_2materials by high-temperature pre-oxidation treatment, resulting in areduced rate of low temperature oxidation. For the alloys of (Mo_(1-x)Nb_x)Si_2and(Mo_(1-x)Nb_x)(Si_(1-y)Al_y)_2, the formation mechanisms of oxidation scale duringhigh-temperature oxidation were established.
Based on the two sublattice model, the theoretical adiabatic temperature of(Mo_(1-x)Nb_x)Si_2and Mo(Si_(1-y)Al_y)_2were simulated, and the results basically tally withthe change trend of the tested highest combustion temperature. Based on the empiricalelectron theory of solids and molecules, the valence electron structure of C11_b typeMeS_2（Me=Mo,Nb；S=Si,Al）was calculated and the changing of properties wasanalyzed. The results indicates that Nb/Al alloying changed the hybridization state ofatoms in C11_b phase, which correspondingly reduces the bond energy of the strongestbond B and the second strongest bond C in C11_b phase, results in the reduction ofhardness. The ratio of covalent valence electron number to total number ofvalence electron of C11_b phase was elevated when alloying with Nb, which isfavorable for improving the strength of C11_b phase, but declined when alloyedwith Al or trace amount of Nb-Al, resulting the decrease of strength.. And most resultsaccords with the properties changing trend of HP alloys.
根据固体与分子经验电子理论，对C11_b型MeS_2（Me=Mo,Nb；S=Si,Al）价电子结构的计算表明，Nb、Al合金化引起C11_b相中原子杂化状态变化，使C11_b相中最强键及次强键的键能及键上共价电子对数的下降，导致宏观硬度降低；Nb单一合金化提高了C11_b相中共价电子数比例值，有利于提高C11_b相的强度；Al单一合金化和微量Nb、Al协同合金化均使值下降，导致C11_b相强度下降。
采用双亚点阵模型对(Mo_(1-x)Nb_x)Si_2和Mo(Si_(1-y)Al_y)_2体系的理论绝热温度进行了模拟计算，结果表明Nb或Al的固溶引起C11_b相和C40相热容及热焓的变化，从而改变体系的绝热温度，实验设计成分(Mo_(1-x)Nb_x)Si_2和Mo(Si_(1-y)Al_y)_2的理论绝热温度均高于1800K，可以在室温下由元素粉末通过燃烧合成反应生成。
以Mo、Si、Nb、Al元素粉末为原料，通过燃烧合成技术制备了(Mo_(1-x)Nb_x)Si_2、Mo (Si_(1-y)Al_y)2和(Mo_(1-x)Nb_x)(Si_(1-y)Al_y)_2合金。燃烧合成产物主要为固溶有Nb(Al)的C11_b相和C40相，存在过饱和固溶现象。Nb合金化促进NbSi_2及MoSi_2型C40相形成，Al单一合金化及Nb、Al协同合金化促进Mo(Si,Al)_2型C40相的形成。Nb、Al合金化促进了MoSi_2燃烧合成反应的放热，使燃烧温度上升，其反应机制为：熔融-溶解-析出。
以燃烧合成产物为原料，分别采用真空热压烧结和放电等离子烧结制备了致密的(Mo_(1-x)Nb_x)Si_2和(Mo_(1-x)Nb_x)(Si_(1-y)Al_y)_2合金，C11_b相中过饱和固溶的Nb/Al在烧结过程中发生脱溶形成C40相。热压使合金相组成趋近于平衡状态。放电等离子烧结速度快、温度低，形成的合金晶粒细小且仍存在过饱和C11_b相。
系统研究了热压合金的室温力学性能，结果表明：少量Nb固溶使(Mo_(1-x)Nb_x)Si_2合金室温硬度下降，弯曲强度升高，对断裂韧性无显著影响。大量Nb使C40相增加，导致硬度上升，强度和断裂韧性下降。Nb和Al协同合金化对室温弯曲强度的影响不大，有Nb存在时，Al添加量达一定值（y=0.15）会显著恶化MoSi_2的强度。少量Nb和Al协同合金化可显著提高室温断裂韧性，最高达到10.7MPa/m~(1/2)，比纯MoSi_2提高了74%，增加合金量促使形成Mo(Si,Al)2型C40相导致(Mo_(1-x)Nb_x)(Si_(1-y)Al_y)_2合金断裂韧性降低而硬度升高。
对放电等离子烧结合金的室温和高温力学性能进行了系统研究，结果表明：放电等离子烧结合金的强度和硬度均高于同成分热压合金。放电等离子烧结(Mo_(1-x)Nb_x)Si_2合金的强度、硬度和断裂韧性变化趋势和热压合金一致，但断裂韧性下降较慢。Nb的增加使(Mo_(1-x)Nb_x)Si_2合金高温压缩强度呈现出先增后降的趋势，(Mo_(0.85)Nb_(0.15))Si_2合金的高温强度达到246MPa，比MoSi_2提高了110%。(Mo_(0.85)Nb_(0.15))Si_2合金高温变形经历了整体变形和玻璃相集中变形两个阶段，玻璃相集中变形使高温流变应力下降，而MoSi_2只经历了整体变形阶段。Nb、Al协同合金化可更有效的改善高温性能，Nb在高温下起到固溶强化作用，并且有助于产生层错强化效应；少量Al可减少晶界SiO2玻璃相使高温强度上升，但大量Al合金化会降低C11_b和C40相的高温强度；(Mo_(0.85)Nb_(0.15)(Si_(0.97)Al_(0.03))_2合金在1400℃具有最高的压缩强度，达到252MPa，该合金同时还具有最佳室温综合力学性能。
热压工艺制备的合金在500℃没有发生粉化瘟疫现象。Nb单一合金化加剧了MoSi_2的低温氧化，通过高温预氧化处理可在(Mo_(1-x)Nb_x)Si_2表面形成保护性氧化膜，提高低温抗氧化性能。Nb和Al协同合金化MoSi_2的低温抗氧化性优于Nb单一合金化，Nb的作用仍然是加速低温氧化，而Al则有利于抑制低温氧化。(Mo_(0.97)Nb_(0.03)(Si_(0.97)Al_(0.03))_2合金低温氧化性能优于纯MoSi_2。大量合金元素不利于高温预氧化保护膜的形成，大量Al促进氧化形成没有自愈合作用的莫来石-氧化铝复合氧化膜，大量Nb促使MoO_3形成，MoO_3在高温下气化，导致氧化膜出现大量孔洞，不能产生保护作用，甚至恶化材料的低温抗氧化性能。
Nb,Al alloyed MoSi_2was synthesized by combustion synthesis in this work. Thecombustion mode, combustion temperature, reaction mechanism, flame-frontpropagation velocity and product structure were investigated. Then dense materialwas prepared by vacuum hot pressing sintering and sparks plasma sintering usingcombustion synthesis products as raw materials. The organizations and propertieswere studied, and the action mechanisms of alloys were clarified.
From the element powders,(Mo_(1-x)Nb_x)Si_2, Mo(Si_(1-y)Al_y)_2and(Mo_(1-x)Nb_x)(Si_(1-y)Al_y)_2alloys were successfully synthesized by the mode ofself-propagating high-temperature synthesis. And the combustion products are formedthrough melting, dissolution and precipitation mechanism in combustion synthesis. Simelts first in alloys without Al, while Al-Si eutectic melt firstly forms after whichSi-rich melt forms in alloys containing Al. Solid Nb and Mo dissolute into the meltwhen contacted with it, and then reaction products precipitate from the supersaturatedsolution.
Using combustion synthesis products as raw materials, dense (Mo_(1-x)Nb_x)Si_2and(Mo_(1-x)Nb_x)(Si_(1-y)Al_y)_2alloy were prepared by vacuum hot pressing sintering and sparkplasma sintering. The precipitation reaction occurs during the sintering process andC40phase forms by Nb/Al precipitate from supersaturated C11_b phase. The phasecomposition of HP alloy is close to the equilibrium state, while saturated C11_bphasecould also be found in the SPS alloys together with tiny grains, because thetemperature is low and time is short in spark plasma sintering process.
For HP alloys, a little Nb solid solution raises the bending strength from216Mpato284MPa, a small amount of Nb and Al co-alloying could significantly increase thefracture toughness at room temperature, up to10.7MPa/m~(1/2), which is74%higherthan pure MoSi_2; but massive alloys promote the formation of C40phase and result inthe decreasing of fracture toughness and increasing of hardness. For SPS alloys,(Mo0.85Nb0.15)(Si_(0.97)Al_(0.03))_2alloy shows the best combination of high-temperaturecompression strength and best room-temperature mechanical properties, and itsstrength at1400℃is252MPa, which is115%higher than pure MoSi_2.
No pesting phenomena were observed in HP alloys when oxidized at at500℃.Nb alloying accelerates the low-temperature oxidation of MoSi_2, while Al isadvantageous for inhibiting oxidation at500℃.(Mo_(0.97)Nb_(0.03)(Si_(0.97)Al_(0.03))_2shows thebest oxidation performance in all alloys. An approach for avoiding low-temperature oxidation was put forward. A glass protective scale can be formed on the surface of(Mo_(1-x)Nb_x)Si_2materials by high-temperature pre-oxidation treatment, resulting in areduced rate of low temperature oxidation. For the alloys of (Mo_(1-x)Nb_x)Si_2and(Mo_(1-x)Nb_x)(Si_(1-y)Al_y)_2, the formation mechanisms of oxidation scale duringhigh-temperature oxidation were established.
Based on the two sublattice model, the theoretical adiabatic temperature of(Mo_(1-x)Nb_x)Si_2and Mo(Si_(1-y)Al_y)_2were simulated, and the results basically tally withthe change trend of the tested highest combustion temperature. Based on the empiricalelectron theory of solids and molecules, the valence electron structure of C11_b typeMeS_2（Me=Mo,Nb；S=Si,Al）was calculated and the changing of properties wasanalyzed. The results indicates that Nb/Al alloying changed the hybridization state ofatoms in C11_b phase, which correspondingly reduces the bond energy of the strongestbond B and the second strongest bond C in C11_b phase, results in the reduction ofhardness. The ratio of covalent valence electron number to total number ofvalence electron of C11_b phase was elevated when alloying with Nb, which isfavorable for improving the strength of C11_b phase, but declined when alloyedwith Al or trace amount of Nb-Al, resulting the decrease of strength.. And most resultsaccords with the properties changing trend of HP alloys.
引文
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