Goncharov Alexander F, Prakapenka Vitali B, Struzhkin Viktor V, Kantor Innokenty, Rivers Mark L, Dalton D Allen
Geophysical Laboratory, Carnegie Institution of Washington, 5251 Broad Branch Rd., NW, Washington, DC 20015, USA.
Rev Sci Instrum. 2010 Nov;81(11):113902. doi: 10.1063/1.3499358.
We have developed in situ x-ray synchrotron diffraction measurements of samples heated by a pulsed laser in the diamond anvil cell at pressure up to 60 GPa. We used an electronically modulated 2-10 kHz repetition rate, 1064-1075 nm fiber laser with 1-100 μs pulse width synchronized with a gated x-ray detector (Pilatus) and time-resolved radiometric temperature measurements. This enables the time domain measurements as a function of temperature in a microsecond time scale (averaged over many events, typically more than 10,000). X-ray diffraction data, temperature measurements, and finite element calculations with realistic geometric and thermochemical parameters show that in the present experimental configuration, samples 4 μm thick can be continuously temperature monitored (up to 3000 K in our experiments) with the same level of axial and radial temperature uniformities as with continuous heating. We find that this novel technique offers a new and convenient way of fine tuning the maximum sample temperature by changing the pulse width of the laser. This delicate control, which may also prevent chemical reactivity and diffusion, enables accurate measurement of melting curves, phase changes, and thermal equations of state.
我们已经开发出一种原位X射线同步加速器衍射测量方法,用于在金刚石对顶砧中对样品进行脉冲激光加热,压力可达60吉帕。我们使用了一台电子调制的2 - 10千赫重复频率、1064 - 1075纳米光纤激光器,其脉冲宽度为1 - 100微秒,并与门控X射线探测器(皮拉图斯探测器)以及时间分辨辐射温度测量装置同步。这使得能够在微秒时间尺度上(对许多事件进行平均,通常超过10000次)进行作为温度函数的时域测量。X射线衍射数据、温度测量以及具有实际几何和热化学参数的有限元计算表明,在当前实验配置下,4微米厚的样品能够以与连续加热相同的轴向和径向温度均匀度水平进行连续温度监测(在我们的实验中可达3000 K)。我们发现,这种新技术提供了一种通过改变激光脉冲宽度来微调样品最高温度的新颖且便捷的方法。这种精确控制还可能防止化学反应性和扩散,从而能够准确测量熔化曲线、相变以及热状态方程。