ZHANG Chao, SUO Tao, TAN Weili, ZHANG Xinyue, WANG Cunxian, LI Yulong. A Method for Testing Dynamic Mechanical Behavior of Materials at Ultra-High Temperature and in-Situ Observation[J]. Chinese Journal of High Pressure Physics, 2018, 32(1): 013202. doi: 10.11858/gywlxb.20170522
Citation: ZHAO Tiejun, WANG Zifa, YAN Honghao, WANG Xiaohong, LI Xiaojie. Dynamic Collection and Micro-Growth Mechanism of TiO2 Nanoparticles in Gaseous Detonation Reaction[J]. Chinese Journal of High Pressure Physics, 2021, 35(5): 053201. doi: 10.11858/gywlxb.20210746

Dynamic Collection and Micro-Growth Mechanism of TiO2 Nanoparticles in Gaseous Detonation Reaction

doi: 10.11858/gywlxb.20210746
  • Received Date: 15 Mar 2021
  • Rev Recd Date: 07 Apr 2021
  • During the preparation of nano TiO2 particles via the gaseous detonation method, a portable nano-powder collection platform was located inside the gaseous detonation tube where the nano-TiO2 powders were collected based on the detonation reaction. The growth mechanism of gaseous detonation preparing nanoparticles was investigated experimentally for the first time. The results demonstrated that the TiO2 powders collected from platform and detonation tube wall consisted of rutile and anatase phases, and the particle size of TiO2 from platform is much smaller than that of tube wall. The particle size was significantly affected by the distance from platform to the end of detonation tube, and the closer the distance, the smaller the TiO2 particle size. The growth mechanism of nanoparticles prepared via gaseous detonation method was revealed based on the theory of detonation/shock wave propagation and experimental observation in detonation tube.

     

  • 泡沫铝作为一种新型功能与结构材料在近几年被广泛应用。其自身独特的多孔结构决定了它具有低密度、高孔隙率和大的比表面积。这些特性使它具有隔音降噪、缓冲吸能等多种作用,被广泛应用于航空航天、国防军事、汽车防护等领域。已有研究表明:泡沫材料在压缩过程中的应力-应变曲线呈现明显的3个阶段,分别是线弹性阶段、塑性平台阶段和密实阶段[1],其中塑性平台阶段是由于胞孔大量坍塌产生的,该过程能够吸收较多的能量,胞孔的破坏模式呈现多样化,因此研究泡沫铝胞孔的破坏模式及微观变形机理对提高泡沫铝的吸能效率有着重要意义。

    泡沫铝变形过程中往往呈现出典型的不均匀压缩特性,利用数字散斑和图像相关方法研究其变形特征具有全场性和直观性等优点[2-3]。魏志强等[4]利用高速摄影技术对泡沫铝的分离式霍普金森压杆(SHPB)实验进行了跟踪拍摄,发现利用图像处理软件分析所得到的应变结果与SHPB后处理得到的应变结果基本一致。Jung等[5]利用数字图像相关法对Ni/Al复合开孔泡沫铝的微观变形进行了研究,发现这种方法可以有效地观察到泡沫铝的微观变形。房亮等[6]通过数字图像相关法研究了闭孔泡沫铝的压缩力学行为,认为闭孔泡沫铝在弹性范围内受压时具有较高的线性度,且发现单个孔的变形特征与孔壁的形态有关。章超等[7]基于数字图像相关法的原理对泡沫铝的冲击压缩过程进行了拍摄跟踪,结果表明在压缩过程中会随机产生多个变形带,形状主要有斜“I”型和“V”型。Kadkhodapour等[8]、杨福俊等[9]在对闭孔泡沫铝变形的研究中发现,泡沫铝的宏观变形受单个胞体变形的影响,且单个胞体的变形模式与胞体的形状以及胞体分布的随机性有关。在泡沫铝研究中以闭孔泡沫铝较多[10-12]。潘艺等[13]认为基体材料和相对密度影响泡沫铝的变形特性,且变形特性也与胞孔分布的随机性有关。Mu等[14]提出胞体的变形与自身的形态有关,且存在4种失效模式。杨宝等[15]通过观察冲击过程中试件的变形图,发现泡沫铝在动态下的破坏模式与准静态下的类似,变形破坏模式有节点旋转变形、悬臂壁弯曲变形、剪切变形破坏、水平曲壁压弯变形以及斜向细孔壁屈曲变形等。

    球形孔开孔泡沫铝由于胞元尺寸和形状统一,在各个方向上的力学性能基本一致,闭孔泡沫铝相对密度较低,且陈永涛等[16]认为相对密度对吸能效率的极值影响较小,并得出闭孔泡沫铝单位体积吸收的能量低于开孔泡沫铝的结论。对开孔泡沫铝应变率效应的研究结果不一:Deshpande[17]、Mukai[18]等的研究表明,开孔泡沫铝对应变率不敏感;程和法等[19]认为泡沫铝的压缩性能具有明显的应变率效应,且应变率越高,吸能效果越好。球形孔开孔泡沫铝由于存在孔壁,兼具通孔和闭孔泡沫铝的特征,可以在某些特殊应用中发挥缓冲耗能的作用。然而,球形孔开孔泡沫铝在压缩载荷下的力学性能、变形特征和细观机理尚不清楚,传统泡沫铝在由变形集中带演化主导的应力平台阶段内材料整体和胞元孔的变形如何影响球形孔泡沫铝的力学行为也亟需研究。基于此,本研究首先针对球形孔开孔泡沫铝的静-动态力学性能进行实验研究,再利用数字图像相关技术对其在准静态压缩下的介观变形机制进行分析。

    实验材料选用北京强业泡沫金属公司提供的球形孔开孔泡沫铝,基体材料为纯铝,采用造孔剂渗流法制备,胞孔直径6 mm,壁面连通孔孔径1~2 mm,试样密度0.9~1.0 g/cm3。静态力学性能实验的试样尺寸为ø30 mm×35 mm,采用电子万能试验机测试。动态力学性能实验分别采用落锤试验机和SHPB,试样尺寸分别为ø30 mm×35 mm和ø30 mm×20 mm。落锤质量约40 kg,冲击高度约1.2 m,锤头上安装加速度传感器测量冲击过程中的加速度,并通过积分换算得到工程应力-应变曲线。SHPB装置杆件直径为50 mm,子弹、入射杆和透射杆长度分别为1.0、2.5和2.5 m,考虑到泡沫材料的透射波信号较弱,采用半导体应变计测量透射波。另外,为研究准静态加载下泡沫铝和胞元孔的具体变形模式,采用GOM 5M三维全场动态测量系统拍摄球形开孔泡沫铝的准静态压缩过程,基于ARAMIS软件对采集图片进行图像处理,获得位移场和应变场信息。实验装置见图1。实验所用两部相机的焦距均为400 mm,分辨率为2 448×2 050像素,标定视场尺寸为44 mm×55 mm。考虑到泡沫铝表面不规则,散斑实验采用矩形试样,尺寸为35 mm×35 mm×35 mm,在观测面喷涂黑白相间随机分布的散斑场(见图2)。加载速率1 mm/min,图像采集间隔为2 s。

    图  1  三维全场应变测量系统
    Figure  1.  Three dimensional full-field strain measurement system
    图  2  泡沫铝试样及喷散斑后试样
    Figure  2.  Foamed aluminum sample and speckle sample

    对泡沫铝力学性能进行分析,图3(a)为准静态压缩过程中泡沫铝的应力-应变曲线,可知:曲线较为光滑平缓,与胞元孔结构和尺寸一致性较高有关;平台阶段较为平稳,主要是由于孔壁厚度较大,胞元孔坍塌时承载能力没有突然降低,体现了球形孔泡沫铝的优点。

    动态实验曲线由相同应变率下3组实验曲线的平均值获得,且取0.05应变下的应力为屈服应力[20]。对比不同应变率下的应力-应变曲线(图3(b))可知,屈服强度在应变率为0.001 s–1时为8.592 MPa,随着应变率的增大,屈服强度增大,在应变率为2 200 s–1时为15.387 MPa,增大了80%。为了定量分析能量吸收特性[20],对比可知20%应变对应的流动应力从14.205 MPa增大到18.236 MPa,提高了28%,吸收能量从2.03 MJ/m3增大到2.78 MJ/m3,增加了40%。文献[21]指出泡沫铝的平台应力接近应变量为0.2时的流动应力,可见该泡沫铝的静、动态力学性能差异显著,存在明显的应变率效应,且动态冲击下泡沫铝具有更高的屈服强度,能吸收更多能量,动态吸能效率的提高说明球形孔泡沫铝具有优异的力学性能,更有利于其作为高速缓冲吸能结构的芯层。

    图4为球形开孔泡沫铝压缩过程位移场,可见,在压缩时间t=173.070 s时(见图4(b))虚线位置出现一条局部变形带,随着加载的进行出现第二条变形带(图4(c)4(d))。局部变形带的产生是泡沫铝胞孔不同形式的坍塌造成的,与胞孔的分布以及孔壁的位置有关,最先发生坍塌的胞孔组成了第一条变形带,这种现象与闭孔泡沫铝相似,都是局部变形带的产生和演化导致材料应力-应变曲线出现典型的平台阶段。由图3中泡沫铝的应力-应变曲线可知,在平台阶段泡沫铝吸收大量能量,这一阶段就是胞孔大量坍塌出现局部变形带的过程。

    图  4  压缩过程泡沫铝表面位移场分布
    Figure  4.  Displacement field distribution of foamed aluminum surface during compression
    图  3  泡沫铝的压缩应力-工程应变曲线
    Figure  3.  Compressive stress-engineering strain curve of aluminum foam

    通过观察与统计胞孔破坏模式,发现胞孔的变形模式主要有3种,如图5所示,其中:图5(a)为孔壁屈曲变形,图5(b)中的孔发生了扭转变形,图5(c)显示在压缩时孔壁既发生扭转变形又存在剪切变形。这与文献[9]中提到的闭孔泡沫铝胞孔的变形模式类似。

    图  5  胞孔的变形模式
    Figure  5.  Deformation mode of cell

    为了分析泡沫铝的介观变形机制,选取单个孔的应变场(图6(a))进行分析。图6(c)为孔的侧面图,可以看出是一个半球形。由该胞孔的应变场(图7)可以看出,在加载时间为173.070 s时,在胞孔壁上的通孔边界处出现一条变形带;继续加载时,在同一起始位置出现第二条变形带,且变形带上应变较大,单个胞孔在压缩变形过程中的应变分布存在很明显的不均匀性。两条变形带的起始位置相同,都是从胞孔上通孔的缺陷处开始,即图6(b)红框中的缺口,且胞孔向后凸起,导致在压缩过程中变形沿着局部变形带发生屈曲;在压缩时间为473.120 s时(见图7(d))缺口变深,胞孔局部变形带就是由于缺口处的应力集中造成的,且多数胞孔情况类似。由此可知,开孔泡沫铝在压缩过程中单个胞体孔壁上由于孔壁缺陷处的应力集中会出现多条变形带,且由于孔壁的凸起,导致胞孔轴向屈曲。

    图  6  单胞孔位置与其孔的侧面应变场
    Figure  6.  Location of the single cell on its surface and lateral strain field map on the side of the celll
    图  7  单胞压缩过程应变场分布
    Figure  7.  Distribution of strain field on the surface of a single cell during compression

    为了分析孔壁的变形模式,选取如图8所示3个厚度不同、方向不同的孔壁组成的区域,单个孔壁呈现“I”型,该结构在泡沫铝中较为普遍,且1区孔壁在变形带处,“I”型孔壁的断裂与破坏直接导致了孔的坍塌变形。在3个孔壁上各选几个点(图8(b)),由分析软件计算出各点的应变-时间曲线,如图9所示。1区上的点既有压应变又有拉应变,在加载时间273.063 s后孔壁有了明显破坏,而在孔壁破坏的过程中,由图9(b)图10(d)都可以看出此时点7有较大的拉应变,达到30%,而点6上压应变较大,因此1区孔壁在破坏过程中受到过较大拉应力,且最终断裂,过程中存在剪切破坏。在153.071 s时,3区上的点1、2、3、4都为压应变,呈线性增大,即孔壁变形模式为孔壁屈曲变形,2区上的点8、9、10处既存在压应变又存在拉应变,且2区在1区孔壁破坏并最终断裂前变形很小,在1区断裂后其变形明显,孔壁上点的拉应变增大,因此可以判断该孔壁是由于1区孔壁破坏造成的扭转与剪切的复合变形。可见在泡沫铝的压缩过程中胞孔的变形模式是由于孔壁变形的多样化造成的,孔壁的变形模式主要有孔壁屈曲变形、剪切、扭转加剪切复合变形3种,最先发生破坏的孔壁变形模式为剪切变形。

    图  8  泡沫铝观测面不同位置孔壁
    Figure  8.  Hole wall at different positions on the observation surface of aluminum foam
    图  9  孔壁各点应变-时间曲线
    Figure  9.  Strain-time curve of each point on the hole wall of foamed aluminum
    图  10  孔壁不同时刻应变场分布
    Figure  10.  Strain field distribution of aluminum foam wall at different time

    经过以上对宏观与介观的分析可以发现,整体变形带的产生与胞孔的变形有关,胞孔的变形模式由孔壁的变形模式决定,孔壁的破坏直接造成了胞孔的坍塌,而胞孔的坍塌又明显地反映出局部变形带的存在。孔壁的3种变形模式决定了胞孔的变形模式,且局部变形带本身由最先发生破坏的孔壁连接而成,对多组实验的统计表明,多条变形带上孔壁的破坏模式以剪切破坏为主。孔壁的变形模式与孔壁的厚度以及方向有关,3种变形模式中剪切变形最不稳定,导致孔壁最先破坏,并出现局部变形带。

    利用三维全场应变测量系统全面分析了球形开孔泡沫铝在准静态压缩下的介观变形,得到以下结论。

    (1)球形孔开孔泡沫铝具有明显的应变率效应,随着应变率的增加,屈服强度增加,平台段提高,且从准静态到应变率为2000 s–1的过程中,应变在0.2时能量吸收增加40%。

    (2)球形孔开孔泡沫铝在细观结构和变形行为上接近于传统闭孔泡沫金属,变形集中带的产生和演化主导了材料的屈服平台阶段行为,局部变形带的产生机理与闭孔泡沫铝类似。

    (3)单个胞体在压缩过程中会在孔壁缺陷处出现局部变形带,且不止一条,主要是由于缺陷位置经过压缩后出现的应力集中造成的。

    (4)胞孔的变形模式主要有3种,屈曲变形、剪切变形、扭转加剪切复合变形;主要由孔壁的3种变形模式决定,孔壁的变形模式与孔壁的厚度以及加载方向有关。

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