JIANG Shuqing, YANG Xue, WANG Yu, ZHANG Xiao, CHENG Peng. Symmetrization and Chemical Precompression Effect of Hydrogen-Bonds in H2-H2O System[J]. Chinese Journal of High Pressure Physics, 2019, 33(2): 020102. doi: 10.11858/gywlxb.20190730
Citation: WANG Bihan, LIN Chuanlong, LIU Xuqiang, YANG Wenge. Phase Transition Kinetics of Ge from dc Phase to β-Sn Phase under High Pressure[J]. Chinese Journal of High Pressure Physics, 2022, 36(2): 021101. doi: 10.11858/gywlxb.20210893

Phase Transition Kinetics of Ge from dc Phase to β-Sn Phase under High Pressure

doi: 10.11858/gywlxb.20210893
  • Received Date: 22 Oct 2021
  • Rev Recd Date: 19 Nov 2021
  • Germanium is a semiconductor with good performances of high carrier mobility and narrow band gap at ambient conditions. Under high pressure, it undergoes serials of polymorphs similar to the case of silicon, and the attractive characteristics in its high pressure phases such as metallization and superconducting transition make it one of the most appealing materials in high pressure research. However, its fundamental phase transition kinetics has been rarely studied. In this work, we present our experimental observations on the phase transition of germanium via a novel designed rapid compression tool and ultrafast time-resolved X-ray diffraction (XRD) acquisition system. The compression rate reaches to tens of TPa/s which is realized by combining gas membrane and piezoceramics compression methods in a symmetrical dynamic diamond anvil cell (dDAC). The time-resolved XRD with high resolution in microseconds is achieved by integrating the high flux pink beam diffraction, an X-ray scintillator to convert diffracted X-rays to visible lights and a high-speed optical camera. It is found that there is a time sequence for diffraction planes disappearing and appearing of dc and β-Sn phases, showing a displacive feature for this phase transition. In addition, the XRD evolution under static compression is also given for comparing with the dynamic compression, the results demonstrate our novel designed rapid compression and ultrafast time-resolved XRD setup shows a great potential for studying the high pressure phase transition kinetics.

     

  • 冲击波加载多孔固体介质过程中形成的极端高温高压条件可激活常规温压条件难以发生的化学反应,为材料合成开辟了一条新途径,尤其是对合成条件苛刻的材料具有显著优势。然而,冲击波作用导致粉末从初始状态至孔隙湮灭的过程中涉及多种机械、物理和化学变化,因而冲击波压缩下的反应过程十分复杂[1]。冲击诱导化学反应取决于外部加载条件和粉末混合物的初始状态等多种因素[2-3],反应物粉末的初始孔隙率是控制冲击反应热力学和动力学的一个非常重要因素[4]。Cooper 等[5]应用理论模拟证实,冲击波和孔隙表面相互作用导致孔隙崩塌产生的大量能量集聚有利于激活化学反应,因此探讨粉末初始孔隙率对诱发超快冲击化学反应的影响极为重要。

    铌硅二元金属间化合物因具有低密度和优良的高温强度等物理特性,可作为潜在的高温结构材料和金属含能材料[6-7]。根据铌-硅二元相图,铌-硅系存在Nb5Si3、Nb3Si和 NbSi2共3种金属间化合物[8]。其中Nb5Si3的熔点(2 515 ℃)最高,密度 (7.16 g/cm3)相对较低,因其具有优良的高温性能受到关注[9]。这类材料的熔点高、晶体结构复杂,采用常规方法难以合成,但该类材料的合成反应能够放热,理论上讲,一旦被激活便可自维持发生反应。由于该激活势垒高,传统方法难以达到激活条件,而冲击波加载产生的极端高温高压对于激活该类反应具有一定优势。目前,已经开展了铌硅化合物的冲击合成工作。Vecchio等[10]应用冲击波加载合成了NbSi2,发现其冲击诱导反应机制与传统固态反应机制不同;Meyers等[11]也通过铌硅粉末混合物的冲击回收,发现塑性变形可以影响铌硅粉末间的反应。此外,还有一些理论模拟研究对铌硅金属间化合物的冲击合成进行探讨[12]。但是,所有铌硅粉末混合物的冲击反应研究,无论是实验结果还是理论分析都仅局限于较低冲击强度条件(飞片速度在2.0 km/s以下),冲击产物也仅获得了较低熔点的NbSi2,而且这些结果对于冲击化学反应的程度和机理解释存在分歧。而且,高熔点金属间化合物(如Nb5Si3)这类传统方法较难合成的材料在高冲击强度范围(飞片速度在2.0 km/s以上)的冲击合成及反应机制未有报道。

    课题组前期开展了铌硅粉末混合物的冲击回收实验,通过高冲击强度下的冲击回收获得了高熔点Nb5Si3化合物[13],发现相同组分配比的铌硅粉末混合物在不同的冲击强度下合成了不同组成的铌硅化合物,且反应特征不同。为更清楚地理解高冲击强度下铌硅粉末混合物的冲击合成及反应机制,在前期工作基础上,本研究进一步对不同孔隙率的铌硅粉末混合物样品进行高冲击强度下回收,通过对冲击回收产物进行表征分析,探讨不同初始孔隙率对铌硅混合物冲击反应的影响。

    实验使用高纯Nb(约325目,Alfa Aesar公司)和Si(约325目,Alfa Aesar公司)粉末原料。将铌粉和硅粉按原子比为5∶3称量,V型混料器中氩气气氛下将粉末混合2 h,通过不同压力将混合好的粉末冷压成直径约为12 mm、厚度约为3 mm的圆片状试样。冲击样品的准备过程(原料称量、混合前的真空封装、压片和铜回收盒的真空封装)均在水氧监测氩气气氛保护的手套箱中完成。将装有样品的铜制回收盒密封。样品孔隙率的计算方法参考文献[14]。

    应用二级轻气炮加载装置对样片进行冲击回收,装置示意图和实物如图1所示。将铜飞片(24 mm × 3.0 mm)粘在发射弹丸上,由磁测速系统测量飞片速度,在飞片速度约2.35 km/s的最高冲击速度下进行冲击回收实验。利用质量平均法计算混合物样品的雨贡纽参数[15-16],采用阻抗匹配法和疏松粉末状态方程计算样品的冲击压力和温度[15,17]表1列出了不同孔隙率粉末混合物的冲击回收实验参数和计算结果。

    图  1  冲击回收实验装置示意图和实物
    Figure  1.  Schematic and photographs of the assembly for the shock recovery experiment
    表  1  不同孔隙度的粉末混合物的冲击回收实验参数
    Table  1.  Shock loading conditions of Nb-Si powder mixtures with different porosity
    SampleFlyer velocity/
    (km·s−1)
    Density/
    (g·cm−3)
    Porosity/
    %
    Shock
    pressure/GPa
    Second shock
    pressure/GPa
    Shock
    temperature/K
    Nb-Si-P15.5051045601 173
    Nb-Si-P22.35 ± 0.024.8952039601 625
    Nb-Si-P33.9803529602 256
    下载: 导出CSV 
    | 显示表格

    图2显示了完整回收的铜回收盒在冲击前、后的外形变化。用机械切割方式从铜制回收盒中将回收的冲击产物分离取出,切掉产物样品外围边缘的含铜部分,留下中心主体部分用于表征分析。将产物样块逐级打磨,并清洗、干燥,储存在真空干燥箱中待表征。

    图  2  冲击回收前、后铜回收盒
    Figure  2.  Copper capsule before and after shock loading

    使用X 射线衍射仪(丹东浩元仪器有限公司,DX-2700型)对样品进行物相表征,采用CuKa 靶(λ = 0.154 06 nm) 射线,衍射角2θ为20°~80°,步长为0.03°,每步计数时间1 s。使用日本电子公司JSM-7001F型场发射扫描电子显微镜 (SEM)进行微观形貌观察,并用SEM配备的能谱仪分析各物相的成分。使用差示扫描量热计(DSC)测量冲击回收产物的热响应曲线(Ar气氛下,加热速率为10 ℃/min)。

    图3为不同孔隙率铌硅粉末冲击产物的XRD图谱。从图3(a)中10%孔隙率冲击样品的XRD结果可见,产物主要为Nb和Si的特征衍射峰及较弱的NbSi2衍射峰,表明仍有大部分Nb和Si未发生反应,仅有极少部分NbSi2相生成。由图3(b)中20%孔隙率铌硅粉末冲击产物的XRD结果可见,该孔隙率产物中虽仍有部分未反应的Nb和Si,但生成NbSi2相的程度有所提高,初始孔隙率提高后,冲击化学反应更易进行。此外,图3(c)中35%孔隙率铌硅粉末混合物的冲击产物XRD图谱显示,其衍射峰仅由Nb5Si3(包括α-Nb5Si3相和β-Nb5Si3相)的特征峰组成。与低孔隙率样品相比,在相同冲击强度下高孔隙率粉末样品更容易获得高熔点Nb5Si3金属间化合物。因此,初始孔隙率对粉末混合物在冲击压缩下物相生成、固相化学反应的影响非常明显。参考表1估算的冲击平均温度也可看出,随着样品初始孔隙率增加,较高的冲击温度(2 256 K)更有利于铌硅金属间化合物发生反应。

    图  3  不同孔隙率铌硅粉末冲击回收产物的XRD 结果
    Figure  3.  XRD patterns of the recycled samples of Nb-Si powder mixtures with different porosity

    图4为10%初始孔隙率铌硅粉末冲击产物的SEM结果,其中图4(b)图4(a)的局部放大图,图4(c)为样品EDS能谱分析结果,w为质量分数。由图4(a)可以看出,样品在该冲击压力(约为45 GPa)下铌硅颗粒被明显压实,没有明显物相生成或发生化学反应。图4(b)中局部区域放大图显示,与初态未冲击样品相比,冲击后的粉末颗粒呈细粒化、等轴状,说明冲击加载作用导致颗粒发生崩裂和相互嵌合。EDS能谱显示图4(b)中亮灰色细粒子的为Nb,周围相对较暗细粒为Si,可能由于NbSi2量极少,在图中未能明确分辨。在较小孔隙率即相对密实的混合反应物样品中,冲击波更多作用于粉末颗粒的机械和物理变形。由于孔隙率低,孔隙崩塌所致的能量贮集弱,极少能够激活并促发冲击化学反应。

    图  4  10%孔隙率铌硅粉末冲击回收产物的SEM结果和EDS分析
    Figure  4.  SEM morphology and EDS spectra of the recycled samples of Nb-Si powder mixtures with the porosity of 10%

    图5为20%初始孔隙率铌硅粉末冲击回收产物的SEM结果,其中图5(b)为图5(a)的局部放大图,图5(c)为样品EDS能谱分析结果。图5(a)中,经冲击加载后20%孔隙率回收产物与10%孔隙率回收产物明显不同,随着冲击作用下温度不断升高,由于Si的熔点较低,而Nb的屈服强度和熔点较高,Si会发生熔融,并分布于变形的Nb周围,与基体特征类似,并且其中弥散着新相。如图5(b)所示,对富Si区域高倍放大观察可见,Si基体中分布着球形、结节状粒子,表现出发生反应的微观特征。对图5(b)方框内粒子进行EDS元素分析发现,其化学组成与NbSi2化学式的原子个数比相符,与XRD结果中出现NbSi2衍射峰一致。由此可见,与10%孔隙率样品相比,在相同飞片速度冲击下,随着冲击温度升高,高初始孔隙率反应产物中的铌硅颗粒发生严重变形并伴随硅发生熔融,并且NbSi2产物增多,表明发生了明显的冲击化学反应。

    图  5  20%孔隙率铌硅粉末冲击回收产物的SEM结果和EDS分析
    Figure  5.  SEM morphology and EDS spectra of the recycled samples of Nb-Si powder mixtures with the porosity of 20%

    图6为高孔隙率(35%)铌硅粉末混合物冲击回收样品的SEM结果。由图6(a)可知,样品已转化为相对均匀的单一微观组织结构,表明该孔隙率样品在相同冲击速度下已发生完全反应形成新的相结构。图6(b)图6(a)中方框内区域局部放大图,图中的新相为枝条状结构,其间有微纳孔(孔隙率约为4.7%,孔隙尺寸介于0.2~4 μm之间)。EDS能谱分析结果显示,铌和硅的原子比约为63.02:36.98,与Nb5Si3化学式的原子个数比接近,表明冲击反应生成物为Nb5Si3化合物。35%孔隙率样品中,冲击加载创造了极高的温度条件(估算冲击样品中的平均温度达2 256 K),相同冲击速度作用于铌硅粉末在物相生成和反应程度上与前述低孔隙率样品相比显著提高,并且其物相形态有明显不同。

    图  6  35%孔隙率铌硅粉末冲击回收产物的SEM结果和EDS分析
    Figure  6.  SEM morphology and EDS spectra of the recycled samples of Nb-Si powder mixtures with the porosity of 35%

    值得注意的是,高孔隙率样品在飞片速度约为2.35 km/s时就发生了完全反应,而前期对不同冲击速度下反应行为的研究发现,较低孔隙率(20%)样品[13]需要更高的冲击速度(飞片速度约为2.63 km/s)才能发生完全反应。因此,高孔隙率样品崩塌所致的高能量贮集产生的高温是发生完全反应的重要条件。

    图7为不同孔隙率铌硅粉末冲击产物的DSC曲线。由图7可知,孔隙率为10%和20%冲击产物的DSC曲线分别在720 ℃和810 ℃附近出现了两个放热峰。结合冲击产物的XRD结果分析可知,720 ℃放热峰可能是冲击产物中未反应的Nb和Si之间进一步发生反应放热所致。可能因为未发生完全化学反应的冲击产物中,未反应的铌和硅粒子在比自蔓延燃烧反应开始温度低约200 ℃时就开始发生化学反应[18]。该异常是由于冲击作用引起粒子粉末发生塑性流动和混合,表面清洁以及样品自身缺陷导致在冲击压缩加载期间粒子粉末被活化。而810 ℃放热峰可能是由于冲击塑变的Nb颗粒发生再结晶。35%孔隙度冲击回收产物的DSC结果呈现光滑的曲线,在测试加热范围内未出现放热峰,表明冲击回收产物为稳定的化合物。这与前述的物相表征和形貌分析结果一致,也证实了35%孔隙度样品完全反应生成了Nb5Si3金属间化合物。

    图  7  不同孔隙率铌硅粉末冲击回收产物的DSC曲线
    Figure  7.  DSC curves of the shock recycled samples of Nb-Si powder mixtures with different porosity

    粉末颗粒混合物的初始状态涵盖颗粒自身组成结构及混合颗粒间的相互接触等条件[19-22]。冲击加载时,在冲击波的高压作用下,样品颗粒的变化不是孤立发生的,而受相互间直接作用和颗粒自身物理性质的限制,表现为样品内颗粒的整体协调变形及交互作用。这些作用对于颗粒的变形方式、变形程度和融合都会产生直接影响。更重要的是,不同变化方式和程度会导致不同的能量集聚,从而产生温度升高和局域热效应[23],这些变化又反过来影响物质的扩散、相互渗透甚至激活化学反应。研究表明[24-25],合适的孔隙率对于粉末颗粒反应物的冲击化学合成非常重要。

    由表征分析结果可知,孔隙率对于铌硅粉末混合物冲击反应的影响,是导致其反应发生及反应机制变化的重要因素。20%孔隙率冲击反应伴随着铌硅颗粒间强烈的相互作用、较低的相互约束以及大面积的孔隙塌陷或湮灭,冲击加热效果显著提升,不仅导致硅粒子发生熔化,变形的铌粒子嵌入到熔融的硅中,而且以铌粒子所在位置为形核中心,铌与周围的硅粒子发生半“固-液”化学反应生成相应的铌硅化合物,不过该激活程度仍处于仅能激发NbSi2反应物生成的条件。在更高孔隙率(35%)下,铌硅颗粒交互作用、变形及孔隙塌陷引起的能量集聚很高,使得样品内部急剧升温,引发高熔点的铌熔化,熔融的铌硅原子发生自由迁移,在极高温度激活下,铌硅间发生“液相”化学反应获得相应的铌硅化合物,即全面激活了铌硅间的自维持反应,并获得高熔点的Nb5Si3金属间化合物且反应完全。值得注意的是,过大孔隙率会在样品中留下微纳尺度孔隙,可能会对样品的块体性能产生影响。此外,实验研究发现,若孔隙率过高,孔隙崩塌产生的过高温度可能使冲击回收样品盒局部熔化,出现破漏或样品内气体相较多导致回收盒爆裂,从而导致冲击回收样品失败。

    通过3种不同初始孔隙率(10%、20%和35%)铌硅粉末混合物的冲击化学反应实验,对冲击回收产物物相、微观形貌表征分析及冲击产物热响应行为进行研究分析,发现不同孔隙率铌硅粉末混合物冲击反应的发生情况、产物特征及反应程度有所不同。低孔隙率(10%)样品几乎不发生反应;当孔隙率提高至20%时,铌硅粉末混合物发生不完全化学反应,生成NbSi2化合物;当孔隙率增大到35%时,相同冲击速度下铌硅粉末混合物发生完全反应,并获得与初始配比一致的Nb5Si3化合物。实验结果证实,适当增大铌硅粉末的初始孔隙率有利于发生冲击化学反应。

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