Igarashi Brian, Christensen Tage, Larsen Ebbe H, Olsen Niels Boye, Pedersen Ib H, Rasmussen Torben, Dyre Jeppe C
DNRF centre Glass and Time, IMFUFA, Department of Sciences, Roskilde University, P.O. Box 260, DK-4000 Roskilde, Denmark.
Rev Sci Instrum. 2008 Apr;79(4):045105. doi: 10.1063/1.2903419.
An experimental setup, including a cryostat and a temperature control system, has been constructed to meet the demands of measuring linear and nonlinear macroscopic relaxation properties of glass-forming liquids in the extremely viscous state approaching the glass transition. In order to be able to measure such frequency-dependent response functions accurately (including dielectric permittivity, specific heat, thermal expansivity, and shear and bulk moduli), as well as nonlinear relaxations following a temperature jump, one must have the ability to hold temperatures of liquids steady over the span of several days or even several weeks. To maximize temperature stability, special care is taken to thermally isolate the sample chamber of the cryostat. The main temperature control system is capable of maintaining temperatures within a few millikelvins. If liquid is deposited into a special transducer assembly that includes a subcryostat unit, the temperature of liquids can be maintained even more precisely, within a few tenths of a millikelvin. This subcryostat unit is more responsive to temperature changes because (i) it is equipped with a Peltier element that provides secondary heating and cooling, (ii) the transducer contains a layer of liquid that is only 50 micfom thick, and (iii) feedback proportional-integral-derivative temperature control is implemented by a fully analog circuit. The subcryostat permits us to change and stabilize temperatures quickly; it takes only 10 s to stabilize the temperature within tenths of a millikelvin after a jump of 1 K, for example, a capability that is highly advantageous for accurately observing relaxation processes following a temperature step.
已构建了一个包括低温恒温器和温度控制系统的实验装置,以满足在接近玻璃化转变的极高粘度状态下测量玻璃形成液体的线性和非线性宏观弛豫特性的需求。为了能够准确测量这种频率相关的响应函数(包括介电常数、比热、热膨胀系数以及剪切模量和体积模量),以及温度跃变后的非线性弛豫,必须具备在几天甚至几周的时间跨度内保持液体温度稳定的能力。为了使温度稳定性最大化,需特别注意对低温恒温器的样品腔进行热隔离。主温度控制系统能够将温度保持在几毫开尔文以内。如果将液体沉积到一个包括低温恒温器单元的特殊换能器组件中,液体温度可以保持得更精确,在十分之几毫开尔文以内。这个低温恒温器单元对温度变化的响应更快,原因如下:(i)它配备了一个提供二次加热和冷却的珀耳帖元件;(ii)换能器包含一层仅50微米厚的液体;(iii)反馈比例积分微分温度控制由一个全模拟电路实现。该低温恒温器使我们能够快速改变和稳定温度;例如,在温度跃升1 K后,只需10秒就能将温度稳定在十分之几毫开尔文以内,这种能力对于精确观察温度阶跃后的弛豫过程非常有利。