CN113281221B - A method and system for measuring the viscosity and surface tension of a high-temperature melt - Google Patents
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Abstract
Description
技术领域technical field
本发明涉及高温熔融体的热物理性质测量方法，具体涉及一种高温熔融体黏度和表面张力的测量方法和系统，属于流体热物理性质测量和表面科学领域。The invention relates to a method for measuring thermophysical properties of a high-temperature melt, in particular to a method and system for measuring the viscosity and surface tension of a high-temperature melt, and belongs to the fields of fluid thermophysical property measurement and surface science.
背景技术Background technique
熔融体的黏度性质是重要的热物理性质，是熔融体工质流动、传热、传质等科学研究及工程应用的关键基础数据。一般地，在低于1000℃条件下，测量熔融体的黏度可选择的方法较多，如振动杯法等；当温度升高，尤其是在2000℃ ~ 3000℃以上时，通过传统的接触测量黏度的方法遇到了困难，很难找到可以适用于这个温区及以上温度的物理探针。传统方法的另外一个问题是：需要采用具有参考数据的标准物质来标定仪器常数，因此是相对的测量方法，一方面参考物质的不确定度会直接叠加至待测样品的黏度不确定度上；另一方面参考物质和待测物质的纯度差异引起的偏差无法估计；对于高温熔融体而言，高温的参考数据较为稀缺，同时测量不确定度一般都比较大。The viscosity property of the melt is an important thermophysical property, and it is the key basic data for scientific research and engineering applications such as working medium flow, heat transfer, and mass transfer of the melt. Generally, when the temperature is lower than 1000°C, there are many methods to measure the viscosity of the melt, such as the vibrating cup method; when the temperature rises, especially when the temperature is above 2000°C ~ 3000°C, it is difficult to measure the viscosity through the traditional contact method, and it is difficult to find a physical probe suitable for this temperature range and above. Another problem with the traditional method is that standard materials with reference data are required to calibrate the instrument constants, so it is a relative measurement method. On the one hand, the uncertainty of the reference material will be directly superimposed on the viscosity uncertainty of the sample to be tested; on the other hand, the deviation caused by the difference in purity between the reference material and the material to be tested cannot be estimated; for high-temperature melts, high-temperature reference data are scarce, and the measurement uncertainty is generally relatively large.
发明内容Contents of the invention
本发明旨在提供一种高温熔融体黏度和表面张力的测量方法和系统，利用表面光散射法测量，可以测量温度范围为600℃ ~ 3000℃内各种熔融体的黏度和表面张力。The present invention aims to provide a method and system for measuring the viscosity and surface tension of high-temperature melts, which can measure the viscosity and surface tension of various melts in the temperature range of 600°C to 3000°C by using the surface light scattering method.
表面光散射法测量高温熔融体的技术特点和优势：（1）绝对测量。全黏度范围内无需标准物质标定，所有输入量均可以实验测得，并且具有清晰的误差传递规律；（2）非接触测量。采用光探针，而非传统方法的物理探针，因此极易拓展至高温、高压等极限条件测量，测量样品池不含运动部件，容易设计。The technical characteristics and advantages of the surface light scattering method for measuring high-temperature melts: (1) Absolute measurement. There is no need for standard material calibration in the full viscosity range, all input quantities can be measured experimentally, and has a clear error transfer law; (2) Non-contact measurement. Optical probes are used instead of physical probes in traditional methods, so it is easy to expand to extreme conditions such as high temperature and high pressure. The measurement sample cell does not contain moving parts and is easy to design.
本发明中，熔融体在相界面处的表面波波长在微米级，振幅在纳米级。当单频激光入射至界面时与表面波相作用，考虑到表面波振幅极小，可以将其视为一个弱光栅，因此在反射光周围会有对应特定波数q（= 2π / λ Λ; λ Λ为表面波波长）的一级衍射光，即散射光。散射光携带有表面波的信息，即频率ω和弛豫时间τ C，利用表面光散射技术即可提出到这两个参数。在特定波数下，表面波的弛豫特性由其色散方程D（ω，τ C，q，σ，ρ L ，η L ，ρ g ，η g ）= 0决定，其中σ，ρ L ，η L ，ρ g ，η g 分别为表面张力，液相密度、黏度，气相密度、黏度。对于熔融体体系，气相参数可以忽略，表面波的弛豫特征一般为过阻尼型，即ω = 0，表面波色散方程为实方程。因此，测量熔融体的黏度η L 需输入参数：液相密度ρ L 和表面张力σ， 这两个参数需要已知，也可以采用躺滴法获得。考虑到熔融体的黏度较高，可以采用色散方程的一阶近似表达式，这时不需液相密度和表面张力即可以获得运动黏度。若已知液体的密度，还可以获得熔融体的表面张力。In the present invention, the wavelength of the surface wave of the melt at the phase interface is at the micron level, and the amplitude is at the nanometer level. When the single-frequency laser is incident on the interface, it interacts with the surface wave. Considering the extremely small amplitude of the surface wave, it can be regarded as a weak grating. Therefore, there will be first-order diffracted light corresponding to a specific wave number q (= 2π / λ Λ ; λ Λ is the wavelength of the surface wave) around the reflected light, that is, scattered light. The scattered light carries the information of the surface wave, that is, the frequency ω and the relaxation time τ C , and these two parameters can be proposed by using the surface light scattering technique. At a specific wave number, the relaxation characteristics of surface waves are determined by their dispersion equation D ( ω , τ C , q , σ , ρ L , η L , ρ g , η g ) = 0, where σ , ρ L , η L , ρ g , η g are surface tension, liquid phase density, viscosity, gas phase density, and viscosity, respectively. For the melt system, the gas phase parameters can be neglected, the relaxation characteristics of the surface wave are generally overdamped, that is, ω = 0 , and the surface wave dispersion equation is a real equation. Therefore, to measure the viscosity η L of the melt, parameters need to be input: liquid phase density ρ L and surface tension σ , these two parameters need to be known, and can also be obtained by the lying drop method. Considering the high viscosity of the melt, the first-order approximate expression of the dispersion equation can be used, and the kinematic viscosity can be obtained without the liquid phase density and surface tension. If the density of the liquid is known, the surface tension of the melt can also be obtained.
本发明提供了一种可以测量高温条件下各种熔融体的黏度和表面张力的测量系统，包括依次连接的激光器、透镜、偏振组合单元、角度测量系统、绝热高温样品池、光纤系统、光电转化模块和数字相关器组成部分。The invention provides a measurement system capable of measuring the viscosity and surface tension of various melts under high temperature conditions, which includes sequentially connected lasers, lenses, polarization combination units, angle measurement systems, adiabatic high temperature sample pools, optical fiber systems, photoelectric conversion modules and digital correlator components.
偏振组合单元包括零级1/2玻片和偏振分光棱镜，透镜依次连接第一高反射镜和零级1/2玻片，零级1/2玻片连接偏振分光棱镜，零级1/2玻片调整线偏振光的偏振方向，偏振分光棱镜将不同偏振的两束光分离；The polarization combination unit includes a zero-order 1/2 glass plate and a polarization beam splitter prism. The lens is sequentially connected to the first high reflection mirror and the zero-order 1/2 glass plate. The zero-order 1/2 glass plate is connected to the polarization beam-splitting prism. The zero-order 1/2 glass plate adjusts the polarization direction of linearly polarized light, and the polarization beam-splitter prism separates two beams of light with different polarizations;
角度测量系统包括垂直方向移动的一维位移台、高精度转台和高反射率反射镜，高反射率反射镜安装在高精度转台上，高精度转台进一步安装在一维位移台上，通过高精度转台调节激光的入射角度，利用垂直方向移动的一维位移台调节激光入射点的位置；The angle measurement system includes a one-dimensional translation stage moving in the vertical direction, a high-precision turntable and a high-reflectivity reflector. The high-reflectivity reflector is installed on a high-precision turntable, and the high-precision turntable is further installed on the one-dimensional translation stage. The incident angle of the laser is adjusted through the high-precision turntable, and the position of the laser incident point is adjusted by the one-dimensional translation stage moving in the vertical direction;
绝热高温样品池包括防辐射真空入射腔、防辐射真空出射腔、主加热器、辅组加热器、保护气进气阀、保护气出气阀和用于真空和气氛控制的阀门；防辐射真空入射腔位于样品池左侧，激光通过该部件入射至样品的表面，样品下部为主加热器，正上方为辅助加热器，经由样品池表面反射的激光通过防辐射真空出射腔射出；样品池在防辐射真空入、出射腔两侧各设有保护气进、出阀；防辐射真空入、出射腔以及样品池上通过阀门连接有抽真空管路，能对样品池内的真空进行控制；The adiabatic high-temperature sample cell includes a radiation-proof vacuum injection chamber, a radiation-proof vacuum exit chamber, a main heater, an auxiliary group heater, a protective gas inlet valve, a protective gas outlet valve, and a valve for vacuum and atmosphere control; the radiation-proof vacuum injection chamber is located on the left side of the sample pool, and the laser is incident on the surface of the sample through this part. The lower part of the sample is the main heater, and the upper part is an auxiliary heater. The inlet and outlet chambers and the sample pool are connected with vacuum pipelines through valves, which can control the vacuum in the sample pool;
光纤系统包括光纤接收器、芯径为100μm的光纤、光纤分光器；光纤接收器与光纤通过FC／ＰＣ方式连接，光纤与光纤分光器利用相同的连接方式连接，构成了光信号由光纤接收器至光纤，后至光纤分光器的通路，光纤分光器将光信号一分为二，两路信号进入光电转化模块；The optical fiber system includes an optical fiber receiver, an optical fiber with a core diameter of 100 μm, and an optical fiber splitter; the optical fiber receiver and the optical fiber are connected by FC/PC, and the optical fiber and the optical fiber splitter are connected by the same connection method, forming a path for the optical signal from the optical fiber receiver to the optical fiber, and then to the optical fiber splitter. The optical fiber splitter divides the optical signal into two, and the two signals enter the photoelectric conversion module;
光电转化模块包括两个光子计数器，并列接受光纤分光器的光信号；The photoelectric conversion module includes two photon counters, which receive the optical signal of the optical fiber splitter in parallel;
数字相关器进一步处理光电转化模块产生的两路电信号，将信号传递给计算机并且进行互相关运算。The digital correlator further processes the two electrical signals generated by the photoelectric conversion module, transmits the signals to the computer and performs cross-correlation calculations.
进一步地，高反射率反射镜安装在一个高精度旋转台上，可以调节探测光的入射角度，高精度转台安装在可以在垂直方向移动的一维位移台上，以确保角度调整后还可以将光束调整至相同的表面位置，Further, the high-reflectivity reflector is installed on a high-precision rotating table, which can adjust the incident angle of the probe light. The high-precision rotating table is installed on a one-dimensional displacement table that can move in the vertical direction, so as to ensure that the beam can be adjusted to the same surface position after angle adjustment.
在高温样品池，两侧设计防辐射真空绝热腔体。样品池的两侧分别设计有两个激光光束的通路，根据入射和出射激光的角度和行程，在通路上设计有防辐射屏和真空控制系统，以减少通过窗口的散射损失。同时还可以对样品池进行真空控制，设计的真空度为10-2 Pa。高温样品池两侧设计有保护气进入和排除口，用于研究不同气氛对于熔融体黏度和表面张力的影响。In the high-temperature sample cell, a radiation-proof vacuum insulation cavity is designed on both sides. Two laser beam passages are designed on both sides of the sample cell. According to the angle and stroke of the incident and outgoing lasers, anti-radiation screens and vacuum control systems are designed on the passages to reduce the scattering loss through the window. At the same time, the vacuum of the sample cell can be controlled, and the designed vacuum degree is 10 -2 Pa. Both sides of the high-temperature sample cell are designed with protective gas inlet and outlet ports, which are used to study the influence of different atmospheres on the viscosity and surface tension of the melt.
样品池为直径为20 mm ~ 40 mm的圆盘，深度为10 mm，材料为陶瓷。样品池底部为主加热器，顶部设计有辅助加热器以防止样品通过对流散射而出现表面冷却，一般地辅助加热器的温度高于主加热器10 ~ 30℃。光纤接收器与光阑之间的距离为40 mm ~ 120 mm。一般地，为了达到良好的测试状态，需确保系统满足外差探测条件，即参考光的光强度为散射光的光强度的40 ~ 100倍。光纤分光器将散射光分为50：50的两路信号，其中一路信号有延迟，采用两个光子计数器进行光电转化，并计算相关量，以防止单光子计数器存在的后脉冲效应。数字相关器一般采用具有线性采样时间的线性相关器或单头相关器，以增加快速表面波时间分辨率。The sample cell is a disc with a diameter of 20 mm to 40 mm, a depth of 10 mm, and the material is ceramic. The bottom of the sample cell is the main heater, and the top is designed with an auxiliary heater to prevent surface cooling of the sample through convective scattering. Generally, the temperature of the auxiliary heater is 10-30°C higher than that of the main heater. The distance between the fiber optic receiver and the diaphragm is 40 mm ~ 120 mm. Generally, in order to achieve a good test status, it is necessary to ensure that the system meets the heterodyne detection conditions, that is, the light intensity of the reference light is 40 to 100 times that of the scattered light. The fiber optic splitter divides the scattered light into two signals of 50:50, one of which has a delay, uses two photon counters for photoelectric conversion, and calculates the relevant quantities to prevent the post-pulse effect of the single photon counter. The digital correlator generally uses a linear correlator or a single-head correlator with a linear sampling time to increase the time resolution of fast surface waves.
本发明提供了一种高温条件下各种熔融体的黏度和表面张力的测量方法，具体的实施方案如下：The invention provides a method for measuring the viscosity and surface tension of various melts under high temperature conditions, and the specific embodiments are as follows:
探测激光为532nm 单纵模线偏振激光器；经过焦距为2m的透镜准直后，通过λ/2波长玻片与偏振分光棱镜组合，同时实现激光光强度和偏振状态的调整，出射光（探测光）的偏振状态为水平偏振，即垂直于纸面；探测光经反射镜入射至高温样品池熔融体表面，并反射至光纤接收器，此时为定义的0°角；反射镜安装在一个高精度旋转台上，可以调节探测光的入射角度，高精度转台安装在可以在垂直方向移动的一维位移台上，以确保角度调整后还可以将光束调整至相同的表面位置，此时光纤接收器接收到的信号为特定散射角度（波数）下的散射光信号，光信号经光纤分光器后分为两路，分别进入两个光子计数器，经过光电转化后进入数字相关器，计算获得的时间相关数据由计算机采集，处理这些数据即可获得特定波数q下，表面波的频率和弛豫时间。The detection laser is a 532nm single longitudinal mode linearly polarized laser; after being collimated by a lens with a focal length of 2m, it passeslambdaThe combination of /2 wavelength glass slide and polarization beam splitter prism realizes the adjustment of laser light intensity and polarization state at the same time. The polarization state of the outgoing light (probe light) is horizontally polarized, that is, perpendicular to the paper surface; the probe light is incident on the surface of the high-temperature sample cell melt through the reflector, and then reflected to the fiber optic receiver, which is at a defined angle of 0°; the reflector is installed on a high-precision rotary table, which can adjust the incident angle of the probe light. The surface position, at this time, the signal received by the optical fiber receiver is the scattered light signal at a specific scattering angle (wavenumber). The optical signal is divided into two paths after passing through the optical fiber splitter, and enters two photon counters respectively, and enters the digital correlator after photoelectric conversion.qBelow, the frequency and relaxation time of the surface wave.
进一步地，激光器采用单模线偏振型，功率为300 mW ~ 2000 mW，出射激光经过焦距为2 m的长焦透镜准直后，利用第一高反射镜3、1/2波长零级玻片4和零级偏振分光棱镜5调整其光强度和偏振状态。一般地，探测光的光强度在几个mW至500 mW之间，取决于熔融体的热物理性质；偏振状态选择为水平偏振，可以在光纤接收器处激发最强的散射光信号。经过强度和偏振状态调制的光束经第二高反射镜和第三高反射镜入射至绝热型-真空、保护气-水冷保护-高温样品池熔融样品13的表面上，然后反射至光纤接收器，此时的入射角度定义为零度角。入射角度及散射角度的控制是通过将第三高反射镜固定在高精度转台上，然后将高精度转台固定在可在垂直方向移动的垂直一维位移台上实现。在实际的测量中，通过选择高精度转台可以调整入射探测光的入射角度，在零角度确定后，可以以零角度为中心调节高精度转台，设置正负两方向上的散射角，根据转台与镜片转动光系，散射角为2倍的高精度转台转动角。一般地，每一个温度下需测量至少三个正负角度信号，结果取平均值。散射光信号经光纤接收器，通过多模光纤至光纤分光器分为两路光信号并产生相位延迟。两路光信号分别经过第一光子计数器和第二光子计数器进行光电转化、信号滤波和放大，并利用数字相关器对信号进行相关运算，进而提取熔融体表面波的弛豫信息，并代入色散方程求解黏度和表面张力。 Furthermore, the laser adopts single-mode linear polarization with a power of 300 mW to 2000 mW. After the outgoing laser is collimated by a telephoto lens with a focal length of 2 m, its light intensity and polarization state are adjusted by using the first high reflection mirror 3, the 1/2 wavelength zero-order glass slide 4 and the zero-order polarization beamsplitter prism 5. Generally, the light intensity of the probe light is between a few mW and 500 mW, depending on the thermophysical properties of the melt; the polarization state is selected as horizontal polarization, which can excite the strongest scattered light signal at the fiber optic receiver. The light beam modulated by intensity and polarization state is incident on the surface of the molten sample 13 of the adiabatic-vacuum, protective gas-water cooling protection-high temperature sample cell through the second high reflective mirror and the third high reflective mirror, and then reflected to the optical fiber receiver. The incident angle at this time is defined as zero degree angle. The control of the incident angle and the scattering angle is realized by fixing the third high-reflection mirror on a high-precision turntable, and then fixing the high-precision turntable on a vertical one-dimensional translation stage that can move in the vertical direction. In actual measurement, the incident angle of the incident probe light can be adjusted by selecting a high-precision turntable. After the zero angle is determined, the high-precision turntable can be adjusted with the zero angle as the center, and the scattering angle in the positive and negative directions can be set. According to the rotating optical system of the turntable and the lens, the scattering angle is twice the rotation angle of the high-precision turntable. Generally, at least three positive and negative angle signals need to be measured at each temperature, and the results are averaged. The scattered light signal is divided into two optical signals through the optical fiber receiver through the multimode fiber to the optical fiber splitter and a phase delay is generated. The two optical signals pass through the first photon counter and the second photon counter for photoelectric conversion, signal filtering and amplification, and use a digital correlator to perform correlation operations on the signals, and then extract the relaxation information of the surface wave of the melt, and substitute it into the dispersion equation to solve the viscosity and surface tension.
测量熔融体黏度和表面张力的精度很大程度取决于温度的控制，为了达到良好的温度控制效果，尤其是抑制通过窗口处的辐射散热，在探测光入射至熔融样品表面的通路上设计了防辐射真空绝热入射腔以缓解高温样品池与窗口的传热，通过真空泵阀门接通真空泵后，利用第一阀门可以对防辐射真空绝热入射腔的真空度进行控制，设计的真空度为10-2Pa；在散射光的通路上设计了防辐射真空绝热出射腔，同样利用真空泵阀门和第二阀门对防辐射真空绝热出射腔的真空度进行控制，同样设计的真空度为10-2Pa。防辐射真空绝热入、出射腔为对称设计，二者的中心轴线与水平面的夹角为10°~ 45°。同时利用真空泵阀门和第三阀门可以对高温样品池的真空度进行控制，设计的真空度为10-2Pa。为了研究不同气氛下熔融体的黏度和表面张力，设计了保护气的净出口通道：保护气进气阀和保护气出气阀。熔融样品下部设计有主加热器，正上方设计有辅助加热器，一般辅助加热器的设定温度较主加热器的温度高10℃ ~ 30℃，以防止熔融体对流散射产生表面冷却。主加热器、辅助加热器以及高温样品池的支持材料均为耐高温陶瓷材料，与高温样品池间采用防辐射屏隔离。为了确保高温样品池光学窗口具有较为准确的角度定位，高温样品池的外壳部分采用钢材料，并利用水冷却保护。The accuracy of measuring melt viscosity and surface tension largely depends on the temperature control. In order to achieve a good temperature control effect, especially to suppress the radiation heat dissipation through the window, a radiation-proof vacuum adiabatic inlet cavity is designed on the path where the probe light is incident on the surface of the molten sample to ease the heat transfer between the high-temperature sample pool and the window. The injection chamber also uses the vacuum pump valve and the second valve to control the vacuum degree of the radiation-proof vacuum adiabatic exit chamber, and the vacuum degree is also designed to be 10 -2 Pa . The radiation-proof vacuum adiabatic inlet and outlet chambers are symmetrically designed, and the angle between the central axis of the two and the horizontal plane is 10°~45°. At the same time, the vacuum degree of the high-temperature sample cell can be controlled by using the vacuum pump valve and the third valve, and the designed vacuum degree is 10 −2 Pa. In order to study the viscosity and surface tension of the melt under different atmospheres, the net outlet channels of the shielding gas are designed: the shielding gas inlet valve and the shielding gas outlet valve. The lower part of the molten sample is designed with a main heater, and the upper part is designed with an auxiliary heater. Generally, the setting temperature of the auxiliary heater is 10°C to 30°C higher than that of the main heater to prevent surface cooling caused by convective scattering of the melt. The supporting materials of the main heater, the auxiliary heater and the high-temperature sample cell are all high-temperature-resistant ceramic materials, and are isolated from the high-temperature sample cell by a radiation shield. In order to ensure that the optical window of the high-temperature sample cell has a more accurate angular positioning, the shell part of the high-temperature sample cell is made of steel and protected by water cooling.
本发明的有益效果：Beneficial effects of the present invention:
该系统测量温度范围为600 ℃ ~ 3000 ℃范围内各种熔融体（透明或不透明均可）的黏度和表面张力，测量标准不确定度分别为2% ~ 5% 和1% ~ 6%。The system measures the viscosity and surface tension of various melts (transparent or opaque) within the temperature range of 600 ℃ ~ 3000 ℃, and the measurement standard uncertainties are 2% ~ 5% and 1% ~ 6%, respectively.
附图说明Description of drawings
图1. 表面光散射法高温熔融体实验系统示意图；Figure 1. Schematic diagram of the high-temperature melt experimental system for the surface light scattering method;
图中：1： 激光器；2：透镜；3：第一高反射镜；4：零级1/2玻片；5：偏振分光棱镜；6：第二高反射镜；7：第三高反射镜；8：一维位移台；9：高精度转台；10：防辐射真空入射腔；11：保护气进气阀；12：保护气出气阀；13：熔融样品；14：高温样品池；15：辅助加热器；16：真空泵阀门；17：第一阀门；18：第二阀门；19：第三阀门；20：防辐射真空出射腔；21：光阑；22光纤接收器；23：光纤；24：光纤分光器；25：第一光子计数器；26：第二光子计数器；27：数字相关器；28：计算机；29：主加热器。In the figure: 1: laser; 2: lens; 3: first high reflective mirror; 4: zero-order 1/2 glass slide; 5: polarization beam splitter prism; 6: second high reflective mirror; 7: third high reflective mirror; 8: one-dimensional translation stage; 9: high-precision turntable; Valve; 18: second valve; 19: third valve; 20: anti-radiation vacuum exit cavity; 21: aperture; 22 optical fiber receiver; 23: optical fiber; 24: optical fiber splitter; 25: first photon counter; 26: second photon counter; 27: digital correlator; 28: computer;
具体实施方式Detailed ways
下面通过实施例来进一步说明本发明，但不局限于以下实施例。The present invention is further illustrated by the following examples, but not limited to the following examples.
实施例1：Example 1:
如图1所示，一种可以测量高温条件下各种熔融体的黏度和表面张力的测量系统，包括依次连接的激光器1、透镜2、偏振组合单元、角度测量系统、绝热高温样品池、光纤系统、光电转化模块和数字相关器组成部分。As shown in Figure 1, a measurement system that can measure the viscosity and surface tension of various melts under high temperature conditions includes a laser 1, a lens 2, a polarization combination unit, an angle measurement system, an adiabatic high-temperature sample cell, an optical fiber system, a photoelectric conversion module, and a digital correlator that are connected in sequence.
偏振组合单元包括零级1/2玻片4和偏振分光棱镜5，透镜2依次连接第一高反射镜3和零级1/2玻片4，零级1/2玻片4连接偏振分光棱镜5，零级1/2玻片4调整线偏振光的偏振方向，偏振分光棱镜5将不同偏振的两束光分离；The polarization combination unit includes a zero-order 1/2 glass plate 4 and a polarization beam splitter prism 5. The lens 2 is sequentially connected to the first high reflection mirror 3 and the zero-order 1/2 glass plate 4. The zero-order 1/2 glass plate 4 is connected to the polarization beam-splitting prism 5. The zero-order 1/2 glass plate 4 adjusts the polarization direction of linearly polarized light, and the polarization beam-splitter prism 5 separates two beams of light with different polarizations;
角度测量系统包括垂直方向移动的一维位移台8、高精度转台9和第三高反射镜7，高反射率反射镜安装在高精度转台上，高精度转台进一步安装在一维位移台上，通过高精度转台调节激光的入射角度，利用垂直方向移动的一维位移台调节激光入射点的位置；The angle measurement system includes a one-dimensional translation stage 8 moving in the vertical direction, a high-precision turntable 9 and a third high-reflection mirror 7. The high-reflectivity reflector is installed on the high-precision turntable, and the high-precision turntable is further installed on the one-dimensional translation stage. The incident angle of the laser is adjusted through the high-precision turntable, and the position of the incident point of the laser is adjusted by the one-dimensional translation stage moving in the vertical direction;
绝热高温样品池包括防辐射真空入射腔10、防辐射真空出射腔20、主加热器29、辅组加热器15、保护气进气阀11、保护气出气阀12和用于真空和气氛控制的阀门；防辐射真空入射腔10位于样品池左侧，激光通过该部件入射至样品的表面，样品下部为主加热器29，正上方为辅助加热器15，经由样品池表面反射的激光通过防辐射真空出射腔20射出；样品池在防辐射真空入、出射腔两侧各设有保护气进、出阀；防辐射真空入、出射腔以及样品池上通过阀门连接有抽真空管路，能对样品池内的真空进行控制；The adiabatic high-temperature sample cell includes a radiation-proof vacuum injection chamber 10, a radiation-proof vacuum exit chamber 20, a main heater 29, an auxiliary heater 15, a shielding gas inlet valve 11, a shielding gas outlet valve 12, and a valve for vacuum and atmosphere control; the radiation-proof vacuum inlet chamber 10 is located on the left side of the sample cell, and the laser is incident on the surface of the sample through this part. There are protective gas inlet and outlet valves on both sides of the radiation vacuum inlet and outlet chambers; the radiation protection vacuum inlet and outlet chambers and the sample pool are connected with vacuum pipelines through valves, which can control the vacuum in the sample pool;
光纤系统包括光纤接收器22、芯径为100μm的光纤23、光纤分光器24；光纤接收器22与光纤23通过FC／ＰＣ方式连接，光纤23与光纤分光器24利用相同的连接方式连接，构成了光信号由光纤接收器至光纤，后至光纤分光器的通路，光纤分光器将光信号一分为二，两路信号进入光电转化模块；The optical fiber system includes an optical fiber receiver 22, an optical fiber 23 with a core diameter of 100 μm, and an optical fiber splitter 24; the optical fiber receiver 22 and the optical fiber 23 are connected by FC/PC, and the optical fiber 23 and the optical fiber splitter 24 are connected by the same connection method, forming a path for the optical signal from the optical fiber receiver to the optical fiber, and then to the optical fiber splitter. The optical fiber splitter divides the optical signal into two, and the two signals enter the photoelectric conversion module;
光电转化模块包括两个光子计数器，并列接受光纤分光器的光信号；The photoelectric conversion module includes two photon counters, which receive the optical signal of the optical fiber splitter in parallel;
数字相关器27进一步处理光电转化模块产生的两路电信号，将信号传递给计算机并且进行互相关运算。The digital correlator 27 further processes the two electrical signals generated by the photoelectric conversion module, transmits the signals to the computer and performs cross-correlation calculations.
进一步地，反射镜安装在一个高精度旋转台上，可以调节探测光的入射角度，高精度转台安装在可以在垂直方向移动的一维位移台上，以确保角度调整后还可以将光束调整至相同的表面位置，Further, the reflector is installed on a high-precision rotating table, which can adjust the incident angle of the probe light. The high-precision rotating table is installed on a one-dimensional displacement table that can move in the vertical direction, so as to ensure that the beam can be adjusted to the same surface position after angle adjustment.
在高温样品池14两侧设计防辐射真空绝热腔体。样品池的两侧分别设计有两个激光光束的通路，根据入射和出射激光的角度和行程，在通路上设计有防辐射屏和真空控制系统，以减少通过窗口的散射损失。同时还可以对样品池进行真空控制，设计的真空度为10-2 Pa。高温样品池两侧设计有保护气进入和排除口，用于研究不同气氛对于熔融体黏度和表面张力的影响。Radiation-proof vacuum insulation chambers are designed on both sides of the high-temperature sample pool 14. Two laser beam passages are designed on both sides of the sample cell. According to the angle and stroke of the incident and outgoing lasers, anti-radiation screens and vacuum control systems are designed on the passages to reduce the scattering loss through the window. At the same time, the vacuum of the sample cell can be controlled, and the designed vacuum degree is 10 -2 Pa. Both sides of the high-temperature sample cell are designed with protective gas inlet and outlet ports, which are used to study the influence of different atmospheres on the viscosity and surface tension of the melt.
样品池为直径为20 mm ~ 40 mm的圆盘，深度为10 mm，材料为陶瓷。样品池底部为主加热器，顶部设计有辅助加热器以防止样品通过对流散射而出现表面冷却，一般地辅助加热器的温度高于主加热器10 ~ 30℃。光纤接收器与光阑之间的距离为40 mm ~ 120 mm。一般地，为了达到良好的测试状态，需确保系统满足外差探测条件，即参考光的光强度为散射光的光强度的40 ~ 100倍。光纤分光器将散射光分为50：50的两路信号，其中一路信号有延迟，采用两个光子计数器进行光电转化，并计算相关量，以防止单光子计数器存在的后脉冲效应。数字相关器一般采用具有线性采样时间的线性相关器或单头相关器，以增加快速表面波时间分辨率。The sample cell is a disc with a diameter of 20 mm to 40 mm, a depth of 10 mm, and the material is ceramic. The bottom of the sample cell is the main heater, and the top is designed with an auxiliary heater to prevent surface cooling of the sample through convective scattering. Generally, the temperature of the auxiliary heater is 10-30°C higher than that of the main heater. The distance between the fiber optic receiver and the diaphragm is 40 mm ~ 120 mm. Generally, in order to achieve a good test status, it is necessary to ensure that the system meets the heterodyne detection conditions, that is, the light intensity of the reference light is 40 to 100 times that of the scattered light. The fiber optic splitter divides the scattered light into two signals of 50:50, one of which has a delay, uses two photon counters for photoelectric conversion, and calculates the relevant quantities to prevent the post-pulse effect of the single photon counter. The digital correlator generally uses a linear correlator or a single-head correlator with a linear sampling time to increase the time resolution of fast surface waves.
本发明提供了一种高温条件下各种熔融体的黏度和表面张力的测量方法，具体的实施方案如下：The invention provides a method for measuring the viscosity and surface tension of various melts under high temperature conditions, and the specific embodiments are as follows:
探测激光为532nm 单纵模线偏振激光器；经过焦距为2m的透镜准直后，通过λ/2波长玻片与偏振分光棱镜组合，同时实现激光光强度和偏振状态的调整，出射光（探测光）的偏振状态为水平偏振，即垂直于纸面；探测光经反射镜入射至高温样品池熔融体表面，并反射至光纤接收器，此时为定义的0°角；反射镜安装在一个高精度旋转台上，可以调节探测光的入射角度，高精度转台安装在可以在垂直方向移动的一维位移台上，以确保角度调整后还可以将光束调整至相同的表面位置，此时光纤接收器接收到的信号为特定散射角度（波数）下的散射光信号，光信号经光纤分光器后分为两路，分别进入两个光子计数器，经过光电转化后进入数字相关器，计算获得的时间相关数据由计算机采集，处理这些数据即可获得特定波数q下，表面波的频率和弛豫时间。The detection laser is a 532nm single longitudinal mode linearly polarized laser; after being collimated by a lens with a focal length of 2m, it passeslambdaThe combination of /2 wavelength glass slide and polarization beam splitter prism realizes the adjustment of laser light intensity and polarization state at the same time. The polarization state of the outgoing light (probe light) is horizontally polarized, that is, perpendicular to the paper surface; the probe light is incident on the surface of the high-temperature sample cell melt through the reflector, and then reflected to the fiber optic receiver, which is at a defined angle of 0°; the reflector is installed on a high-precision rotary table, which can adjust the incident angle of the probe light. The surface position, at this time, the signal received by the optical fiber receiver is the scattered light signal at a specific scattering angle (wavenumber). The optical signal is divided into two paths after passing through the optical fiber splitter, and enters two photon counters respectively, and enters the digital correlator after photoelectric conversion.qBelow, the frequency and relaxation time of the surface wave.
进一步地，激光器1采用单模线偏振型，功率为300 mW ~ 2000 mW，出射激光经过焦距为2 m的长焦透镜2准直后，利用第一高反射镜3、零级1/2玻片4和零级偏振分光棱镜5调整其光强度和偏振状态。一般地，探测光的光强度在几个mW至500 mW之间，取决于熔融体的热物理性质；偏振状态选择为水平偏振，可以在光纤接收器22处激发最强的散射光信号。经过强度和偏振状态调制的光束经第二高反射镜6和第三高反射镜7入射至绝热型-真空、保护气-水冷保护-高温样品池14熔融样品13的表面上，然后反射至光纤接收器22，此时的入射角度定义为零度角。入射角度及散射角度的控制是通过将第三高反射镜7固定在高精度转台9上，然后将高精度转台固定在可在垂直方向移动的垂直一维位移台8上实现。在实际的测量中，通过选择高精度转台9可以调整入射探测光的入射角度，在零角度确定后，可以以零角度为中心调节高精度转台，设置正负两方向上的散射角，根据转台与镜片转动关系，散射角为2倍的高精度转台9转动角。一般地，每一个温度下需测量至少三个正负角度信号，结果取平均值。散射光信号经光纤接收器22，通过多模光纤23至光纤分光器24分为两路光信号并产生相位延迟。两路光信号分别经过第一光子计数器25和第二光子计数器26进行光电转化、信号滤波和放大，并利用数字相关器27对信号进行相关运算，进而提取熔融体表面波的弛豫信息，并代入色散方程求解黏度和表面张力。 Further, the laser 1 adopts a single-mode linear polarization type, with a power of 300 mW to 2000 mW. After the outgoing laser is collimated by a telephoto lens 2 with a focal length of 2 m, the light intensity and polarization state are adjusted by the first high reflection mirror 3, the zero-order 1/2 glass slide 4 and the zero-order polarization beam splitter prism 5. Generally, the light intensity of the probe light is between several mW and 500 mW, depending on the thermophysical properties of the melt; The light beam modulated by intensity and polarization state is incident on the surface of the adiabatic-vacuum, protective gas-water cooling protection-high temperature sample cell 14 molten sample 13 through the second high reflective mirror 6 and the third high reflective mirror 7, and then reflected to the optical fiber receiver 22, and the incident angle at this time is defined as zero degree angle. The control of the incident angle and the scattering angle is realized by fixing the third high-reflection mirror 7 on the high-precision turntable 9, and then fixing the high-precision turntable on the vertical one-dimensional translation stage 8 that can move in the vertical direction. In actual measurement, the incident angle of the incident probe light can be adjusted by selecting the high-precision turntable 9. After the zero angle is determined, the high-precision turntable can be adjusted with the zero angle as the center, and the scattering angle in the positive and negative directions can be set. According to the rotation relationship between the turntable and the lens, the scattering angle is twice the rotation angle of the high-precision turntable 9. Generally, at least three positive and negative angle signals need to be measured at each temperature, and the results are averaged. The scattered optical signal passes through the optical fiber receiver 22, passes through the multimode optical fiber 23 to the optical fiber splitter 24, and is divided into two optical signals and generates a phase delay. The two optical signals pass through the first photon counter 25 and the second photon counter 26 for photoelectric conversion, signal filtering and amplification, and use the digital correlator 27 to perform correlation calculations on the signals, and then extract the relaxation information of the surface wave of the melt, and substitute it into the dispersion equation to solve the viscosity and surface tension.
测量熔融体黏度和表面张力的精度很大程度取决于温度的控制，为了达到良好的温度控制效果，尤其是抑制通过窗口处的辐射散热，在探测光入射至熔融样品13表面的通路上设计了防辐射真空绝热入射腔10以缓解高温样品池14与窗口的传热，通过真空泵阀门16接通真空泵后，利用第一阀门17可以对防辐射真空绝热入射腔10的真空度进行控制，设计的真空度为10-2Pa；在散射光的通路上设计了防辐射真空出射腔20，同样利用真空泵阀门16和第二阀门18对防辐射真空绝热出射腔20的真空度进行控制，同样设计的真空度为10- 2Pa。防辐射真空绝热入、出射腔为对称设计，二者的中心轴线与水平面的夹角为10°~ 45°。同时利用真空泵阀门16和第三阀门19可以对高温样品池14的真空度进行控制，设计的真空度为10-2Pa。为了研究不同气氛下熔融体的黏度和表面张力，设计了保护气的净出口通道：保护气进气阀11和保护气出气阀12。熔融样品13下部设计有主加热器29，正上方设计有辅助加热器15，一般辅助加热器的设定温度较主加热器的温度高10℃ ~ 30℃，以防止熔融体对流散射产生表面冷却。主加热器、辅助加热器以及高温样品池的支持材料均为耐高温陶瓷材料，与高温样品池14间采用防辐射屏隔离。为了确保高温样品池光学窗口具有较为准确的角度定位，高温样品池的外壳部分采用钢材料，并利用水冷却保护。测量熔融体黏度和表面张力的精度很大程度取决于温度的控制，为了达到良好的温度控制效果，尤其是抑制通过窗口处的辐射散热，在探测光入射至熔融样品13表面的通路上设计了防辐射真空绝热入射腔10以缓解高温样品池14与窗口的传热，通过真空泵阀门16接通真空泵后，利用第一阀门17可以对防辐射真空绝热入射腔10的真空度进行控制，设计的真空度为10 -2 Pa；在散射光的通路上设计了防辐射真空出射腔20，同样利用真空泵阀门16和第二阀门18对防辐射真空绝热出射腔20的真空度进行控制，同样设计的真空度为10 - 2 Pa。 The radiation-proof vacuum adiabatic inlet and outlet chambers are symmetrically designed, and the angle between the central axis of the two and the horizontal plane is 10°~45°. At the same time, the vacuum degree of the high-temperature sample cell 14 can be controlled by using the vacuum pump valve 16 and the third valve 19, and the designed vacuum degree is 10 −2 Pa. In order to study the viscosity and surface tension of the melt under different atmospheres, the net outlet channel of the shielding gas is designed: the shielding gas inlet valve 11 and the shielding gas outlet valve 12 . The lower part of the molten sample 13 is designed with a main heater 29, and an auxiliary heater 15 is designed directly above it. Generally, the set temperature of the auxiliary heater is 10°C to 30°C higher than that of the main heater to prevent surface cooling caused by convection and scattering of the melt. The supporting materials of the main heater, the auxiliary heater and the high-temperature sample cell are all high-temperature-resistant ceramic materials, and are isolated from the high-temperature sample cell 14 by a radiation-proof screen. In order to ensure that the optical window of the high-temperature sample cell has a relatively accurate angular positioning, the shell part of the high-temperature sample cell is made of steel and protected by water cooling.
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