锆基块体金属玻璃合金化及半固态处理研究
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摘要
块体金属玻璃（BMG）具有优异的力学性能和物理性能，为新型结构材料和功能材料的发展开辟了新的领域。然而，BMG在室温下发生灾难性脆性断裂，已经成为制约该材料规模化工程应用的瓶颈。因此，寻找提高BMG塑性的途径是目前研究的热点问题。本文针对BMG发展中的主要问题，以BMG合金化和半固态处理为主要研究目的，以不含贵重金属元素及有毒元素Be的Zr基低成本BMG合金为研究对象开展了以下几个主要方面的研究:
1.研究了制备条件对Zr基BMG热稳定性和力学性能的影响。在相同的冷却速度下，通过改变铸造条件，考察热速处理、浇注保温时间、浇注温度对BMG热稳定性和力学性能的影响，以确定最佳的制备条件。结果表明，热速处理可以增加BMG的GFA和热稳定性，对于Zr_(55)Al_(10)Ni_5Cu_(30)BMG，当铸造电压从7kV提高至10kV时，过冷液相区△Tx和参数γ分别从73K增至89K，从0.413增至0.417。在加热温度及冷却速率等条件不变的情况下，随着浇注保温时间的延长，瞬态形核率增大，液态合金有结晶的趋势，原子的排列也由无规向有序转变趋势，结构无序密堆性下降，非晶合金的GFA和热稳定性降低。在相同的冷却速率和浇注温度下，制备BMG的浇注保温时间存在一个临界值，超过此临界值，试样开始晶化。高的浇注温度制备的非晶合金GFA和压缩断裂强度增加，塑性下降。对于特定成分的BMG，存在一个最佳的浇注温度，即在此浇注温度条件下制备的BMG的压缩断裂强度最高，塑性最好，BMG的力学性能在一定程度上可由浇注温度控制。在相同的铸造条件下，考察了不同成分试样合金的冷却速度对BMG的GFA和力学性能的影响，结果表明，相同的冷却速度对不同成分合金的GFA和力学性能的影响不同，与大直径BMG相比，具有相同化学成分的小尺寸的BMG表现出更为优异的塑性和良好的压缩断裂强度。
2.选择Zr_(55)Cu_(30)Ni_5Al_(10)BMG作为基体合金，研究了Fe、Mn、Nb元素合金化对其热稳定性和力学性能的影响，并讨论其作用机理。结果表明，元素加入对合金非晶形成有一定的成分范围，当含量达到极限值时，在相同的冷却条件下，加入组元与原有组元之间很可能发生反应形成晶体相。Fe元素的添加使得非晶合金的GFA呈现先增加后降低的趋势，热稳定性呈现下降的趋势。Fe元素添加量为1%时，可以提高非晶合金的GFA，其约化玻璃转变温度Trg为0.59，参数γ为0.414。添加过量的Fe元素（4%的Fe含量），会导致基体合金晶化，形成非晶与晶体的复合材料。添加2%的Fe元素，其BMG的压缩断裂强度和塑性应变分别为1868MPa和2.62%，表现了良好的综合力学性能。添加4%的Mn元素能形成Ф3mm的BMG，非晶合金的热稳定性和GFA呈现下降趋势，其过冷液相区△Tx为61K，约化玻璃转变温度Trg为0.58，参数γ为0.40，压缩断裂强度为1817MPa，塑性无明显改善。添加适量的Nb能提高基体合金的热稳定性和GFA。当Nb含量为8%时，BMG具有最好的热稳定性和最高的GFA，其过冷液相区ΔTx值达到86K，参数γ达到0.416。Nb元素的适量添加有利于提高非晶合金的压缩断裂强度和塑性变形能力，(Zr0.55Al0.1Ni0.05Cu0.3)92Nb8BMG的压缩断裂强度和塑性应变分别达到1877MPa和1.92%。
3.通过改变铸造电压（熔化功率），进而改变熔化温度，使母合金达到固-液两相区，通过改变半固态温度和保温时间，研究了半固态温度和半固态保温时间对先析出的金属间化合物相尺寸形貌、分布、体积分数的影响及其与复合材料力学性能之间的关系，并讨论了复合材料的增塑机制。研究表明，半固态温度升高，(Zr_(0.55)Al_(0.10)Ni_(0.05)Cu_(0.30))_(96)Fe_4BMG复合材料的GFA增加，析出的金属间化合物第二相的体积分数减小。在铸造电压7kV时制备出具有室温压缩塑性的铸态内生球形金属间化合物/BMG复合材料，其不但具有高的压缩断裂强度（达到2203MPa），也具有显著的室温塑性（塑性变形达到5.85%）。半固态温度对(Zr_(0.55)Al_(0.10)Ni_(0.05)Cu_(0.30))_(96)Fe_4BMG复合材料中析出的金属间化合物第二相的微观形态有着很大的影响。铸造电压7kV制备的合金试样非晶基体上分布着球形金属间化合物，其直径大部分在10μm-20μm之间，体积分数为45.3%。复合材料中球形金属间化合物相与非晶基体之间界面清晰，未发现其它相的出现。TEM研究表明球形金属间化合物相与玻璃基体之间具有较好的界面结合力，有效的解决了湿润性的问题，低能量的界面使球形金属间化合物第二相与基体之间牢固而稳定地结合。压缩变形后的试样表面出现了大量的波浪状的多重剪切带，呈现出隆起现象，其间距都小于1μm，小于球形金属间化合物第二相的尺寸。在合适的合金成分下，可以通过半固态温度的调整获得铸态内生球形金属间化合物/BMG两相微观组织，与相应的单相BMG比较，可以在有效的提高材料塑性的同时保持高的断裂强度，有利于获得更好的综合力学性能。延长半固态保温时间，(Zr_(0.55)Al_(0.10)Ni_(0.05)Cu_(0.30))_(94)Fe_6BMG复合材料晶化明显，GFA降低；随着半固态保温时间的延长，试样中析出的金属间化合物第二相的体积分数增大。(Zr_(0.55)Al_(0.10)Ni_(0.05)Cu_(0.30))_(94)Fe_6BMG复合材料的力学性能与金属间化合物第二相的体积分数密切相关，延长半固态保温时间，金属间化合物第二相的体积分数增大，合金试样的压缩断裂强度和塑性应变呈明显的下降趋势。
Bulk metallic glasses (BMG) with excellent mechanical and physical propertiesopen a new research field for structural and functional materials. However thecatastrophic brittle fracture at room temperature has restricted the extensiveapplication of BMG. Extensive effort have been devoted to the finding of new methodfor improving the ductility in BMG. In this paper, based on the main developmentissues in BMG, Zr-based BMG which have not precious metals and toxic elements Beare selected to study the influences of alloying and semi-solid processing on BMG, thefollows are the main conclusions:
The effects of the preparation conditions on thermal stability and mechanicalproperties of Zr-based BMG were investigated. By changing the casting conditions,the effects of thermal rate treatment, casting holding time and casting temperature onthermal stability and mechanical properties of BMG were studied under the samecooling rate, thus the optimal preparation conditions were determined. The resultsshow that thermal rate treatment can increase GFA and thermal stability of the BMG,for Zr_(55)Al_(10)Ni_5Cu_(30)BMG, supercooled liquid region△Txand parameter γ increasefrom73K to89K, from0.413to0.417, respectively, as casting voltage increase from7kV to10kV. Under the same heating temperature and cooling rates, the transientnucleation rate and the crystallization trend of liquid melt increase with castingholding time increase. And the random arrangement of atoms change to the orderarrangement, the disordered close-packed structure, GFA and thermal stabilitydecrease. There is a critical value of casting holding time in BMG under the samecooling rate and casting temperature, beyond this critical value, the samples begin tocrystallize. GFA and compression fracture strength increase, compressive plasticitydecrease with casting temperature increase. There is an optimum casting temperatureto the specific composition of BMG. Compression fracture strength and compressiveplasticity increase under the optimum casting temperature. Mechanical properties tosome extents are controlled by casting temperature. The influence of cooling rate ofthe different component samples on GFA and mechanical properties were investigatedunder the same casting conditions. The results show that there are different influencesof different composition samples on GFA and mechanical properties under the samecooling rate, and large-diameter BMG, compared with the same chemical compositionof the small-diameter BMG show more excellent compression plasticity and compression fracture strength.
Selected Zr_(55)Al_(10)Ni_5Cu_(30)BMG as the base alloy to study effects and mechanismof adding Fe, Mn, Nb elements on thermal stability and mechanical properties. Theresults show that addition element content of forming amorphous alloy has a certainlimit addition content. When addition content reaches the limit value, it is likely toreact between addition element and original group elements and form crystal phaseunder the same cooling conditions. Adding Fe makes the GFA of BMG increase atfirst and then decrease, thermal stability decrease. Fe addition content is1%, canimprove GFA, reduced glass transition temperature Trgis0.59, parameter γ is0.414.Excessive Fe addition content (4%Fe content) results in crystallization of amorphousmatrix, forming amorphous matrix composite. Fe addition content is2%, the samplehave an excellent mechanical properties, that is, BMG's compression fracture strengthand plastic strain are1868MPa and2.62%, respectively. Mn addition content is4%,can form BMG which the critical dimension is Ф3mm, thermal stability and GFAdecrease, supercooled liquid region△Txis61K, reduced glass transition temperatureTrgis0.58, parameter γ is0.40, compression fracture strength is1817MPa, has noductility. Adding the appropriate amount of Nb element can improve thermal stabilityand GFA. When Nb addition content is8%, BMG has the best thermal stability andthe highest GFA, supercooled liquid region△Txreaches to86K, parameter γ reachesto0.416. Also Nb addition content is8%, the sample has an excellent mechanicalproperties, that is, BMG's compression fracture strength and plastic strain are1877MPa and1.92%, respectively.
By changing casting voltage(heating power), thereby changing heatingtemperature, making master alloy temperature enter to solid-liquid two phase region,to study the effects of semi-solid temperature and holding time on precipitatedintermetallic phases appearance, distribution, volume fraction and the relationshipwith mechanical properties of BMG's composite. Also the enhancement ductilitymechanism was discussed. It show GFA of (Zr0.55Al0.10Ni0.05Cu0.30)96Fe4BMGcomposites increase and precipitated intermetallic second phase volume fractiondecrease with semi-solid temperature increase. As-cast in-situ spherical intermetallicphase/BMG composite which has room temperature compress plasticity wassuccessfully prepared at casting voltage7kV. The BMG composites not only has highcompression fracture strength (reaches2203MPa), but also has significant roomtemperature ductility (plastic strain reaches5.85%). Semi-solid temperature has a great influence on BMG composite precipitated intermetallic second phasemorphology. At casting voltage7kV, BMG composite precipitated intermetallicsecond phase morphology is spherical, most of them are10μm-20μm diameter,volume fraction is45.3%, interface between the amorphous matrix, find no otherphases appear. TEM studies have shown that spherical intermetallic phase and theglass substrate has a better interface binding force, effectively solve the wettingproblem, low-energy interface has a strong and stable binding force between sphericalintermetallic phase and the glass substrate. After deformed, the sample surface showsa large number of waved multiple shear bands which pitch is less than1μm, is lessthan the spherical size of the intermetallic second phase. Under the appropriate alloycomposition, semi-solid temperature can be adjusted to obtain as-cast in-situ sphericalintermetallic phase/BMG composite, with the corresponding single-phase BMGcomparison, can effectively improve the plasticity of the material while maintaininghigh compression fracture strength. GFA of (Zr0.55Al0.10Ni0.05Cu0.30)94Fe6BMGcomposites decrease and precipitated intermetallic second phase volume increase withsemi-solid holding time increase. There is a closely relation between mechanicalproperties and intermetallic second phase volume fraction of(Zr_(0.55)Al_(0.10)Ni_(0.05)Cu_(0.30))_(94)Fe_6BMG composites. Precipitated intermetallic secondphase volume increase, compression fracture strength and plastic strain decease withsemi-solid holding time increase.
1.研究了制备条件对Zr基BMG热稳定性和力学性能的影响。在相同的冷却速度下，通过改变铸造条件，考察热速处理、浇注保温时间、浇注温度对BMG热稳定性和力学性能的影响，以确定最佳的制备条件。结果表明，热速处理可以增加BMG的GFA和热稳定性，对于Zr_(55)Al_(10)Ni_5Cu_(30)BMG，当铸造电压从7kV提高至10kV时，过冷液相区△Tx和参数γ分别从73K增至89K，从0.413增至0.417。在加热温度及冷却速率等条件不变的情况下，随着浇注保温时间的延长，瞬态形核率增大，液态合金有结晶的趋势，原子的排列也由无规向有序转变趋势，结构无序密堆性下降，非晶合金的GFA和热稳定性降低。在相同的冷却速率和浇注温度下，制备BMG的浇注保温时间存在一个临界值，超过此临界值，试样开始晶化。高的浇注温度制备的非晶合金GFA和压缩断裂强度增加，塑性下降。对于特定成分的BMG，存在一个最佳的浇注温度，即在此浇注温度条件下制备的BMG的压缩断裂强度最高，塑性最好，BMG的力学性能在一定程度上可由浇注温度控制。在相同的铸造条件下，考察了不同成分试样合金的冷却速度对BMG的GFA和力学性能的影响，结果表明，相同的冷却速度对不同成分合金的GFA和力学性能的影响不同，与大直径BMG相比，具有相同化学成分的小尺寸的BMG表现出更为优异的塑性和良好的压缩断裂强度。
2.选择Zr_(55)Cu_(30)Ni_5Al_(10)BMG作为基体合金，研究了Fe、Mn、Nb元素合金化对其热稳定性和力学性能的影响，并讨论其作用机理。结果表明，元素加入对合金非晶形成有一定的成分范围，当含量达到极限值时，在相同的冷却条件下，加入组元与原有组元之间很可能发生反应形成晶体相。Fe元素的添加使得非晶合金的GFA呈现先增加后降低的趋势，热稳定性呈现下降的趋势。Fe元素添加量为1%时，可以提高非晶合金的GFA，其约化玻璃转变温度Trg为0.59，参数γ为0.414。添加过量的Fe元素（4%的Fe含量），会导致基体合金晶化，形成非晶与晶体的复合材料。添加2%的Fe元素，其BMG的压缩断裂强度和塑性应变分别为1868MPa和2.62%，表现了良好的综合力学性能。添加4%的Mn元素能形成Ф3mm的BMG，非晶合金的热稳定性和GFA呈现下降趋势，其过冷液相区△Tx为61K，约化玻璃转变温度Trg为0.58，参数γ为0.40，压缩断裂强度为1817MPa，塑性无明显改善。添加适量的Nb能提高基体合金的热稳定性和GFA。当Nb含量为8%时，BMG具有最好的热稳定性和最高的GFA，其过冷液相区ΔTx值达到86K，参数γ达到0.416。Nb元素的适量添加有利于提高非晶合金的压缩断裂强度和塑性变形能力，(Zr0.55Al0.1Ni0.05Cu0.3)92Nb8BMG的压缩断裂强度和塑性应变分别达到1877MPa和1.92%。
3.通过改变铸造电压（熔化功率），进而改变熔化温度，使母合金达到固-液两相区，通过改变半固态温度和保温时间，研究了半固态温度和半固态保温时间对先析出的金属间化合物相尺寸形貌、分布、体积分数的影响及其与复合材料力学性能之间的关系，并讨论了复合材料的增塑机制。研究表明，半固态温度升高，(Zr_(0.55)Al_(0.10)Ni_(0.05)Cu_(0.30))_(96)Fe_4BMG复合材料的GFA增加，析出的金属间化合物第二相的体积分数减小。在铸造电压7kV时制备出具有室温压缩塑性的铸态内生球形金属间化合物/BMG复合材料，其不但具有高的压缩断裂强度（达到2203MPa），也具有显著的室温塑性（塑性变形达到5.85%）。半固态温度对(Zr_(0.55)Al_(0.10)Ni_(0.05)Cu_(0.30))_(96)Fe_4BMG复合材料中析出的金属间化合物第二相的微观形态有着很大的影响。铸造电压7kV制备的合金试样非晶基体上分布着球形金属间化合物，其直径大部分在10μm-20μm之间，体积分数为45.3%。复合材料中球形金属间化合物相与非晶基体之间界面清晰，未发现其它相的出现。TEM研究表明球形金属间化合物相与玻璃基体之间具有较好的界面结合力，有效的解决了湿润性的问题，低能量的界面使球形金属间化合物第二相与基体之间牢固而稳定地结合。压缩变形后的试样表面出现了大量的波浪状的多重剪切带，呈现出隆起现象，其间距都小于1μm，小于球形金属间化合物第二相的尺寸。在合适的合金成分下，可以通过半固态温度的调整获得铸态内生球形金属间化合物/BMG两相微观组织，与相应的单相BMG比较，可以在有效的提高材料塑性的同时保持高的断裂强度，有利于获得更好的综合力学性能。延长半固态保温时间，(Zr_(0.55)Al_(0.10)Ni_(0.05)Cu_(0.30))_(94)Fe_6BMG复合材料晶化明显，GFA降低；随着半固态保温时间的延长，试样中析出的金属间化合物第二相的体积分数增大。(Zr_(0.55)Al_(0.10)Ni_(0.05)Cu_(0.30))_(94)Fe_6BMG复合材料的力学性能与金属间化合物第二相的体积分数密切相关，延长半固态保温时间，金属间化合物第二相的体积分数增大，合金试样的压缩断裂强度和塑性应变呈明显的下降趋势。
Bulk metallic glasses (BMG) with excellent mechanical and physical propertiesopen a new research field for structural and functional materials. However thecatastrophic brittle fracture at room temperature has restricted the extensiveapplication of BMG. Extensive effort have been devoted to the finding of new methodfor improving the ductility in BMG. In this paper, based on the main developmentissues in BMG, Zr-based BMG which have not precious metals and toxic elements Beare selected to study the influences of alloying and semi-solid processing on BMG, thefollows are the main conclusions:
The effects of the preparation conditions on thermal stability and mechanicalproperties of Zr-based BMG were investigated. By changing the casting conditions,the effects of thermal rate treatment, casting holding time and casting temperature onthermal stability and mechanical properties of BMG were studied under the samecooling rate, thus the optimal preparation conditions were determined. The resultsshow that thermal rate treatment can increase GFA and thermal stability of the BMG,for Zr_(55)Al_(10)Ni_5Cu_(30)BMG, supercooled liquid region△Txand parameter γ increasefrom73K to89K, from0.413to0.417, respectively, as casting voltage increase from7kV to10kV. Under the same heating temperature and cooling rates, the transientnucleation rate and the crystallization trend of liquid melt increase with castingholding time increase. And the random arrangement of atoms change to the orderarrangement, the disordered close-packed structure, GFA and thermal stabilitydecrease. There is a critical value of casting holding time in BMG under the samecooling rate and casting temperature, beyond this critical value, the samples begin tocrystallize. GFA and compression fracture strength increase, compressive plasticitydecrease with casting temperature increase. There is an optimum casting temperatureto the specific composition of BMG. Compression fracture strength and compressiveplasticity increase under the optimum casting temperature. Mechanical properties tosome extents are controlled by casting temperature. The influence of cooling rate ofthe different component samples on GFA and mechanical properties were investigatedunder the same casting conditions. The results show that there are different influencesof different composition samples on GFA and mechanical properties under the samecooling rate, and large-diameter BMG, compared with the same chemical compositionof the small-diameter BMG show more excellent compression plasticity and compression fracture strength.
Selected Zr_(55)Al_(10)Ni_5Cu_(30)BMG as the base alloy to study effects and mechanismof adding Fe, Mn, Nb elements on thermal stability and mechanical properties. Theresults show that addition element content of forming amorphous alloy has a certainlimit addition content. When addition content reaches the limit value, it is likely toreact between addition element and original group elements and form crystal phaseunder the same cooling conditions. Adding Fe makes the GFA of BMG increase atfirst and then decrease, thermal stability decrease. Fe addition content is1%, canimprove GFA, reduced glass transition temperature Trgis0.59, parameter γ is0.414.Excessive Fe addition content (4%Fe content) results in crystallization of amorphousmatrix, forming amorphous matrix composite. Fe addition content is2%, the samplehave an excellent mechanical properties, that is, BMG's compression fracture strengthand plastic strain are1868MPa and2.62%, respectively. Mn addition content is4%,can form BMG which the critical dimension is Ф3mm, thermal stability and GFAdecrease, supercooled liquid region△Txis61K, reduced glass transition temperatureTrgis0.58, parameter γ is0.40, compression fracture strength is1817MPa, has noductility. Adding the appropriate amount of Nb element can improve thermal stabilityand GFA. When Nb addition content is8%, BMG has the best thermal stability andthe highest GFA, supercooled liquid region△Txreaches to86K, parameter γ reachesto0.416. Also Nb addition content is8%, the sample has an excellent mechanicalproperties, that is, BMG's compression fracture strength and plastic strain are1877MPa and1.92%, respectively.
By changing casting voltage(heating power), thereby changing heatingtemperature, making master alloy temperature enter to solid-liquid two phase region,to study the effects of semi-solid temperature and holding time on precipitatedintermetallic phases appearance, distribution, volume fraction and the relationshipwith mechanical properties of BMG's composite. Also the enhancement ductilitymechanism was discussed. It show GFA of (Zr0.55Al0.10Ni0.05Cu0.30)96Fe4BMGcomposites increase and precipitated intermetallic second phase volume fractiondecrease with semi-solid temperature increase. As-cast in-situ spherical intermetallicphase/BMG composite which has room temperature compress plasticity wassuccessfully prepared at casting voltage7kV. The BMG composites not only has highcompression fracture strength (reaches2203MPa), but also has significant roomtemperature ductility (plastic strain reaches5.85%). Semi-solid temperature has a great influence on BMG composite precipitated intermetallic second phasemorphology. At casting voltage7kV, BMG composite precipitated intermetallicsecond phase morphology is spherical, most of them are10μm-20μm diameter,volume fraction is45.3%, interface between the amorphous matrix, find no otherphases appear. TEM studies have shown that spherical intermetallic phase and theglass substrate has a better interface binding force, effectively solve the wettingproblem, low-energy interface has a strong and stable binding force between sphericalintermetallic phase and the glass substrate. After deformed, the sample surface showsa large number of waved multiple shear bands which pitch is less than1μm, is lessthan the spherical size of the intermetallic second phase. Under the appropriate alloycomposition, semi-solid temperature can be adjusted to obtain as-cast in-situ sphericalintermetallic phase/BMG composite, with the corresponding single-phase BMGcomparison, can effectively improve the plasticity of the material while maintaininghigh compression fracture strength. GFA of (Zr0.55Al0.10Ni0.05Cu0.30)94Fe6BMGcomposites decrease and precipitated intermetallic second phase volume increase withsemi-solid holding time increase. There is a closely relation between mechanicalproperties and intermetallic second phase volume fraction of(Zr_(0.55)Al_(0.10)Ni_(0.05)Cu_(0.30))_(94)Fe_6BMG composites. Precipitated intermetallic secondphase volume increase, compression fracture strength and plastic strain decease withsemi-solid holding time increase.
引文
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