Zr/Al基非晶合金的电阻及内耗行为与熔体状态的相关性
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摘要
非晶合金通常需快速冷却获得，其短程有序而长程无序的结构与液态合金结构有很大的相似性，因此非晶态组织在很大程度上是母合金熔体的“冻结”，母合金熔体的结构变化必然影响到非晶的形成和性能。本文采用电阻法和内耗法，系统地研究了非晶的形成能力(GFA)、力学弛豫以及晶化行为与熔体状态的关系。论文工作所获得的主要研究成果与认知如下：
(1)选取Al_(86)Ni_9La_5合金作为研究对象，通过电阻法发现其熔体在1320K~1490K温度范围内出现了异常温度变化行为，提示此合金熔体发生了温度诱导的液-液结构转变，这一现象和推测得到了DTA热分析结果的验证。根据不同熔体状态的区间选择合适的温度制备了一系列非晶薄带，连续升温及等温实验研究表明，虽然最终晶化产物并无差异，熔体状态对合金不同阶段的晶化行为却产生了显著的影响。具体表现为：高温熔体制备的非晶，其初生相α-Al的析出温度略有提前，而二级晶化相Al_(11)La_3、Al_3Ni、Al_4La及Al_3Ni_2的析出温度则显著推迟。这些结果对Al基非晶/纳米晶复合材料的制备方法及性能提高有重要意义，也间接印证了在1320K~1490K范围发生液液结构转变的推测。分析认为，熔体状态改变后形成非晶的二级晶化相析出推迟，可归因于其熔体中对应于这些金属间化合物结构和成分的化学短程序得以消散，故这些金属间化合物相从非晶中形核析出更加困难。
(2)对于技术上难以测定熔体电阻率的锆基Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)合金，采用不同熔体温度制备其非晶合金，间接探索了不同熔体结构与性质的状态变化及其对其晶化行为的影响。研究表明，低于1573K温度制备的非晶，其初生相是Ni_2Zr_3；而高于1573K温度制备的非晶，初生相主要是f.c.c NiZr_2，且电阻及DSC实验表明其晶化开始温度Tx提高。更为有趣的是，熔体温度还导致其非晶最终晶化产物的不同。这些结果不仅澄清了文献报道中关于Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)晶化相不一致的原因，同时可推测，当熔体温度超过某一临界值时（介于1573K与1673K之间），Ni-Zr类型的团簇的打破使得熔体结构改变，间接证明了合金熔体中温度诱导液液结构转变的发生。
(3)研究结果揭示，随合金系统的差异，不同熔体温度及其状态变化可导致对GFA的完全相反的影响。对于上述两种合金，Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)合金随制备温度的上升（尤其温度高于1573K之后），表征GFA的特征参数ΔTx、Trg以及γ都明显增大，表明其非晶形成能力增大；而对于Al_(86)Ni_9La_5合金，表征GFA的特征参数以及实际形成非晶临界尺寸均表明，高温熔体（状态改变后）的非晶形成能力有一定程度的下降。
(4)关于非晶制备熔体温度对GFA的作用，对于高温所致氧化及冷速变慢的负面作用，以及高温使得熔体中异质形核基底消散等正面作用，无疑需根据合金系统、制备工艺条件、原材料等方面进行综合分析。而作者基于研究结果分析强调认为：就熔体结构状态本身而言，液液结构转变导致熔体某些原有团簇的消失，若这些团簇的局域结构和成分对应于熔体冷却过程的先析出相（结晶），则必然提高GFA，如Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)合金，推断高温下对应于Ni_2Zr_3的化学短程序的打破；相反地，若消散的局域有序团簇并不对应于晶化和结晶过程的先析出相，且反而在热力学和/或动力学方面有利于先析相的晶核形成，则必然降低GFA，如Al_(86)Ni_9La_5合金，分析认为熔体转变导致化学短程序的消散释放出更多Al原子，从而富Al的原子团簇增多，且熔体的自由体积增大（密度降低）有益于扩散，两方面促进合金先析相α-Al的形核。
(5)采用内耗法探索熔体温度对Zr_(55)Al_(10)Ni_5Cu_(30)大块非晶力学弛豫行为影响的结果表明，随着熔体温度的升高，对应非晶试样的内耗峰向高温移动，且内耗峰值增大。通过比较内耗-频率谱可知，在从室温到晶化开始温度之前，内耗频率关系分别呈现为线性正比、复杂过渡及单调减小，表现出滞弹性和粘弹性两种力学弛豫行为。制备非晶时的熔体温度越高，由滞弹性弛豫转变为粘弹性弛豫的开始温度以及结束温度越低。为了分析玻璃转变温度附近的内耗行为，根据Perez理论和与主弛豫相关的低频内耗表达式，比较了表征非晶物质中短程有序度的参数，发现不同温度制备的非晶其确定的关联参数大小不同，1603K制备的非晶合金的关联参数最大，且由关联参数确定的临界温度点Ti随着制备非晶温度的升高而升高，表明制备非晶的熔体温度越高，非晶越无序，试样热稳定性最好。
(6)选择具有不同非晶形成能力的锆基非晶，研究了非晶形成能力和内耗的关系。通过比较内耗温度曲线发现不同非晶形成能力在内耗峰峰高上有显著区别，GFA越大，内耗峰峰值越高，从而提出了一个表征GFA的新参数—内耗峰峰值。通过对背底内耗拟合获得了激活能，发现非晶形成能力越大，在玻璃转变之前以及过冷液相区的激活能越大。
The amorphous alloys are generally obtained by rapidly cooling. The short-range order andlong-range disorder of amorphous alloy has similarity with the melt structure. So the amorphousalloy might be considered as the solids with the frozen-in liquid structure and some features of meltstructure could be inherited by the resultant amorphous alloy. In the present work, by the methods ofelectrical resistance (ER) and internal friction, the influences of melt temperature on the glassforming ability (GFA), crystallization behavior and mechanical relaxation of the amorphous alloyswere systematically studied. The innovative points and main results of this paper are listed below.
(1) The structure change of the Al_(86)Ni_9La_5liquid was examined by means of ER duringcontinuous heating. Abnormal behaviors with temperature of the melts were observed within therange from1320K to1490K, indicating the change of the liquid state and the possible temperatureinduced liquid-liquid structure transition (LLST). The results also have been verified by DTA. Basedon the anomalous behavior of temperature-induced liquid-liquid structure transition observed in themelt, different melt temperatures were chosen to prepare the amorphous samples and then they wereannealed at the same conditions. It is found that the final crystallization phases are the same, but thecrystallization behavior during different crystallization stages are significantly different among thesamples. For the crystallization behavior of the sample prepared above the LLST temperature range,the precipitation temperature of primary phase α-Al is earlier, but the formation of intermetalliccompounds is later than that of the sample prepared below the LLST temperature. These conclusionscould improve the preparation and performance of Al-based amorphous/nanocrystalline compositematerial, and also indirectly confirm the speculation of liquid-liquid structural change. The resultthat the precipitation of second crystallization of amorphous sample prepared above the LLSTtemperature range, may be attributed to the dissolved short-range order corresponding to theseintermetallic compounds. Therefore, the nucleation and precipitation of the intermetallic compoundsis more difficult.
(2) For the Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)amorphous alloys, it is difficult to measure ER of melt because oftheir proneness to be easily oxidized. So based on the crystallization behavior of amorphous ribbonsprepared at different melt temperatures, the structural change in the melt is indirectly explored. Itwas found that primary phase is different among the samples. The primary phase is Ni_2Zr_3for thesample prepared below1573K, while that is f.c.c NiZr_2for the sample prepared at above1573K,and the begging crystallization temperature moves to higher temperature. The final crystallizationphases are also different for the two kinds of the samples. So based on the signficant differentcrystallization behaviors of amorphous Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)ribbons prepared at different melt temperatures, the reason that crystallization phases reported in some literatures are inconsistentmight originate from the different structures of the amorphous ribbons resulting from different melttemperatures. Besides, it also suggested that the structure of melt changed above1573K.
(3) For different alloy system, the melt structure has significant influence on GFA. Bycomparing the characteristic parameters of GFA Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)ribbons, the GFA is improvedwith the increasing melt temperature, especially higher than1573K. But for Al_(86)Ni_9La_5alloy, basedon the characteristic parameters of GFA and the critical thickness of the wedge-shaped samplesprepared at diifferent melt temperature, the GFA is decreased due to the change of the melt structure.
(4) For the influence of the quenching temperature on the GFA of the metallic glasses, it is nodoubt to conduct a comprehensive analysis of the negative effects, i.e. the high-temperatureoxidation and the cooling rate slowing down and the positive effects, i.e. high temperature meltmakes the heterogeneous nucleation substrate to dissipate, according to the aspects such as the alloysystem, preparation condition and raw materials. Based on the research results, the authorsemphasize that the liquid-liquid structure transition causes some of the pre-existing clustersdisappearing as the melt structure state itself. If the local structure and composition of the cluster arecorresponding to the primary phase during the rapid cooling of the melt, the GFA will be certainlyimproved. As an example of Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)alloy, it is corresponding to the chemical short rangeorder of Ni_2Zr_3which is broken under the high melt temperature. On the contrary, if the disappearedcluster is not corresponding to the primary phase during crystallization and instead of facilitating thenucleation of the primary phase in the aspects of thermodynamic and/or kinetic, the GFA will becertainly decreased. As an example of Al_(86)Ni_9La_5alloy, the liquid-liquid structure transition causethe disappearing of the chemical short-range order and much more Al atoms will be free resulting inthe increasing of the Al-rich cluster. Meantime, the increasing free volume of the melt (lower density)is favor of the atomic diffusion. Both of the factors promote the nucleation of the primary phasefcc-Al of the alloy.
(5) By the method of internal friction, the influence of melt temperature on the mechanicalrelaxation of Zr_(55)Al_(10)Ni_5Cu_(30)bulk metallic glass was studied. By comparing the internal friction-temperature curves of different samples, the positions of peak move to higher temperature and thethe internal friction value increases with the melt temperature increasing. By comparing the internalfriction-frequency curves of different samples, BMGs structure relaxation can be divided into threeregions before Tx, which are the stages of linear increase, complicated transition and monotonereducing. The beginning and end temperature at which the anelastic behaviour change intoviscoelastic relaxation move toward the lower temperature for the BMG prepared at higher melttemperature. In order to analyze the IF behavior of BMG in the vicinity of the glass transition temperature, based on the theory of Perez, the correlation parameter is compared, which isdeduced from tan-f curves. The sample prepared at1603K has the largest. And the criticaltemperature determined by the correlation parameter increases with the quenching temperatureincerasing. The results show that the higher the melt temperature, the larger the degree of disorder ofthe sample and thus the higher the thermal stability.
(6) Finally, the Zr-based BMGs with different glass forming ability were selected to study therelationship between GFA and internal friction. By comparing the internal friction-temperaturecurves of different samples, it is found that the higher the value of internal friction peak, the betterthe GFA. So a new criterion evaluating the GFA is proposed, i.e. internal friction peak. Comparingthe activation energy obtained from the fitted background internal friction, the higher the glassforming ability, the larger the activation energy before the glass transition temperature and in thesupercooled liquid region.
(1)选取Al_(86)Ni_9La_5合金作为研究对象，通过电阻法发现其熔体在1320K~1490K温度范围内出现了异常温度变化行为，提示此合金熔体发生了温度诱导的液-液结构转变，这一现象和推测得到了DTA热分析结果的验证。根据不同熔体状态的区间选择合适的温度制备了一系列非晶薄带，连续升温及等温实验研究表明，虽然最终晶化产物并无差异，熔体状态对合金不同阶段的晶化行为却产生了显著的影响。具体表现为：高温熔体制备的非晶，其初生相α-Al的析出温度略有提前，而二级晶化相Al_(11)La_3、Al_3Ni、Al_4La及Al_3Ni_2的析出温度则显著推迟。这些结果对Al基非晶/纳米晶复合材料的制备方法及性能提高有重要意义，也间接印证了在1320K~1490K范围发生液液结构转变的推测。分析认为，熔体状态改变后形成非晶的二级晶化相析出推迟，可归因于其熔体中对应于这些金属间化合物结构和成分的化学短程序得以消散，故这些金属间化合物相从非晶中形核析出更加困难。
(2)对于技术上难以测定熔体电阻率的锆基Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)合金，采用不同熔体温度制备其非晶合金，间接探索了不同熔体结构与性质的状态变化及其对其晶化行为的影响。研究表明，低于1573K温度制备的非晶，其初生相是Ni_2Zr_3；而高于1573K温度制备的非晶，初生相主要是f.c.c NiZr_2，且电阻及DSC实验表明其晶化开始温度Tx提高。更为有趣的是，熔体温度还导致其非晶最终晶化产物的不同。这些结果不仅澄清了文献报道中关于Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)晶化相不一致的原因，同时可推测，当熔体温度超过某一临界值时（介于1573K与1673K之间），Ni-Zr类型的团簇的打破使得熔体结构改变，间接证明了合金熔体中温度诱导液液结构转变的发生。
(3)研究结果揭示，随合金系统的差异，不同熔体温度及其状态变化可导致对GFA的完全相反的影响。对于上述两种合金，Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)合金随制备温度的上升（尤其温度高于1573K之后），表征GFA的特征参数ΔTx、Trg以及γ都明显增大，表明其非晶形成能力增大；而对于Al_(86)Ni_9La_5合金，表征GFA的特征参数以及实际形成非晶临界尺寸均表明，高温熔体（状态改变后）的非晶形成能力有一定程度的下降。
(4)关于非晶制备熔体温度对GFA的作用，对于高温所致氧化及冷速变慢的负面作用，以及高温使得熔体中异质形核基底消散等正面作用，无疑需根据合金系统、制备工艺条件、原材料等方面进行综合分析。而作者基于研究结果分析强调认为：就熔体结构状态本身而言，液液结构转变导致熔体某些原有团簇的消失，若这些团簇的局域结构和成分对应于熔体冷却过程的先析出相（结晶），则必然提高GFA，如Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)合金，推断高温下对应于Ni_2Zr_3的化学短程序的打破；相反地，若消散的局域有序团簇并不对应于晶化和结晶过程的先析出相，且反而在热力学和/或动力学方面有利于先析相的晶核形成，则必然降低GFA，如Al_(86)Ni_9La_5合金，分析认为熔体转变导致化学短程序的消散释放出更多Al原子，从而富Al的原子团簇增多，且熔体的自由体积增大（密度降低）有益于扩散，两方面促进合金先析相α-Al的形核。
(5)采用内耗法探索熔体温度对Zr_(55)Al_(10)Ni_5Cu_(30)大块非晶力学弛豫行为影响的结果表明，随着熔体温度的升高，对应非晶试样的内耗峰向高温移动，且内耗峰值增大。通过比较内耗-频率谱可知，在从室温到晶化开始温度之前，内耗频率关系分别呈现为线性正比、复杂过渡及单调减小，表现出滞弹性和粘弹性两种力学弛豫行为。制备非晶时的熔体温度越高，由滞弹性弛豫转变为粘弹性弛豫的开始温度以及结束温度越低。为了分析玻璃转变温度附近的内耗行为，根据Perez理论和与主弛豫相关的低频内耗表达式，比较了表征非晶物质中短程有序度的参数，发现不同温度制备的非晶其确定的关联参数大小不同，1603K制备的非晶合金的关联参数最大，且由关联参数确定的临界温度点Ti随着制备非晶温度的升高而升高，表明制备非晶的熔体温度越高，非晶越无序，试样热稳定性最好。
(6)选择具有不同非晶形成能力的锆基非晶，研究了非晶形成能力和内耗的关系。通过比较内耗温度曲线发现不同非晶形成能力在内耗峰峰高上有显著区别，GFA越大，内耗峰峰值越高，从而提出了一个表征GFA的新参数—内耗峰峰值。通过对背底内耗拟合获得了激活能，发现非晶形成能力越大，在玻璃转变之前以及过冷液相区的激活能越大。
The amorphous alloys are generally obtained by rapidly cooling. The short-range order andlong-range disorder of amorphous alloy has similarity with the melt structure. So the amorphousalloy might be considered as the solids with the frozen-in liquid structure and some features of meltstructure could be inherited by the resultant amorphous alloy. In the present work, by the methods ofelectrical resistance (ER) and internal friction, the influences of melt temperature on the glassforming ability (GFA), crystallization behavior and mechanical relaxation of the amorphous alloyswere systematically studied. The innovative points and main results of this paper are listed below.
(1) The structure change of the Al_(86)Ni_9La_5liquid was examined by means of ER duringcontinuous heating. Abnormal behaviors with temperature of the melts were observed within therange from1320K to1490K, indicating the change of the liquid state and the possible temperatureinduced liquid-liquid structure transition (LLST). The results also have been verified by DTA. Basedon the anomalous behavior of temperature-induced liquid-liquid structure transition observed in themelt, different melt temperatures were chosen to prepare the amorphous samples and then they wereannealed at the same conditions. It is found that the final crystallization phases are the same, but thecrystallization behavior during different crystallization stages are significantly different among thesamples. For the crystallization behavior of the sample prepared above the LLST temperature range,the precipitation temperature of primary phase α-Al is earlier, but the formation of intermetalliccompounds is later than that of the sample prepared below the LLST temperature. These conclusionscould improve the preparation and performance of Al-based amorphous/nanocrystalline compositematerial, and also indirectly confirm the speculation of liquid-liquid structural change. The resultthat the precipitation of second crystallization of amorphous sample prepared above the LLSTtemperature range, may be attributed to the dissolved short-range order corresponding to theseintermetallic compounds. Therefore, the nucleation and precipitation of the intermetallic compoundsis more difficult.
(2) For the Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)amorphous alloys, it is difficult to measure ER of melt because oftheir proneness to be easily oxidized. So based on the crystallization behavior of amorphous ribbonsprepared at different melt temperatures, the structural change in the melt is indirectly explored. Itwas found that primary phase is different among the samples. The primary phase is Ni_2Zr_3for thesample prepared below1573K, while that is f.c.c NiZr_2for the sample prepared at above1573K,and the begging crystallization temperature moves to higher temperature. The final crystallizationphases are also different for the two kinds of the samples. So based on the signficant differentcrystallization behaviors of amorphous Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)ribbons prepared at different melt temperatures, the reason that crystallization phases reported in some literatures are inconsistentmight originate from the different structures of the amorphous ribbons resulting from different melttemperatures. Besides, it also suggested that the structure of melt changed above1573K.
(3) For different alloy system, the melt structure has significant influence on GFA. Bycomparing the characteristic parameters of GFA Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)ribbons, the GFA is improvedwith the increasing melt temperature, especially higher than1573K. But for Al_(86)Ni_9La_5alloy, basedon the characteristic parameters of GFA and the critical thickness of the wedge-shaped samplesprepared at diifferent melt temperature, the GFA is decreased due to the change of the melt structure.
(4) For the influence of the quenching temperature on the GFA of the metallic glasses, it is nodoubt to conduct a comprehensive analysis of the negative effects, i.e. the high-temperatureoxidation and the cooling rate slowing down and the positive effects, i.e. high temperature meltmakes the heterogeneous nucleation substrate to dissipate, according to the aspects such as the alloysystem, preparation condition and raw materials. Based on the research results, the authorsemphasize that the liquid-liquid structure transition causes some of the pre-existing clustersdisappearing as the melt structure state itself. If the local structure and composition of the cluster arecorresponding to the primary phase during the rapid cooling of the melt, the GFA will be certainlyimproved. As an example of Zr_(65)Al_(7.5)Ni_(10)Cu_(17.5)alloy, it is corresponding to the chemical short rangeorder of Ni_2Zr_3which is broken under the high melt temperature. On the contrary, if the disappearedcluster is not corresponding to the primary phase during crystallization and instead of facilitating thenucleation of the primary phase in the aspects of thermodynamic and/or kinetic, the GFA will becertainly decreased. As an example of Al_(86)Ni_9La_5alloy, the liquid-liquid structure transition causethe disappearing of the chemical short-range order and much more Al atoms will be free resulting inthe increasing of the Al-rich cluster. Meantime, the increasing free volume of the melt (lower density)is favor of the atomic diffusion. Both of the factors promote the nucleation of the primary phasefcc-Al of the alloy.
(5) By the method of internal friction, the influence of melt temperature on the mechanicalrelaxation of Zr_(55)Al_(10)Ni_5Cu_(30)bulk metallic glass was studied. By comparing the internal friction-temperature curves of different samples, the positions of peak move to higher temperature and thethe internal friction value increases with the melt temperature increasing. By comparing the internalfriction-frequency curves of different samples, BMGs structure relaxation can be divided into threeregions before Tx, which are the stages of linear increase, complicated transition and monotonereducing. The beginning and end temperature at which the anelastic behaviour change intoviscoelastic relaxation move toward the lower temperature for the BMG prepared at higher melttemperature. In order to analyze the IF behavior of BMG in the vicinity of the glass transition temperature, based on the theory of Perez, the correlation parameter is compared, which isdeduced from tan-f curves. The sample prepared at1603K has the largest. And the criticaltemperature determined by the correlation parameter increases with the quenching temperatureincerasing. The results show that the higher the melt temperature, the larger the degree of disorder ofthe sample and thus the higher the thermal stability.
(6) Finally, the Zr-based BMGs with different glass forming ability were selected to study therelationship between GFA and internal friction. By comparing the internal friction-temperaturecurves of different samples, it is found that the higher the value of internal friction peak, the betterthe GFA. So a new criterion evaluating the GFA is proposed, i.e. internal friction peak. Comparingthe activation energy obtained from the fitted background internal friction, the higher the glassforming ability, the larger the activation energy before the glass transition temperature and in thesupercooled liquid region.
引文
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