CN106442228A - Device for measuring surface tension by using high-temperature melt maximum bubble method - Google Patents

Device for measuring surface tension by using high-temperature melt maximum bubble method Download PDF

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CN106442228A
CN106442228A CN201610655866.5A CN201610655866A CN106442228A CN 106442228 A CN106442228 A CN 106442228A CN 201610655866 A CN201610655866 A CN 201610655866A CN 106442228 A CN106442228 A CN 106442228A
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temperature
surface tension
melt
capillary
furnace
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吕学伟
严志明
陈赟
邓青宇
徐健
党杰
张颖异
张文娟
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Chongqing University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N13/02Investigating surface tension of liquids
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N13/02Investigating surface tension of liquids
    • G01N2013/0225Investigating surface tension of liquids of liquid metals or solder
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N13/02Investigating surface tension of liquids
    • G01N2013/0241Investigating surface tension of liquids bubble, pendant drop, sessile drop methods
    • G01N2013/0266Bubble methods

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Abstract

本发明提供了一种高温熔体最大气泡法测表面张力的装置,它包括气体输送及控制系统、加热炉、升降系统、气氛控制系统置、温度控制系统和控制系统。气体输送及控制系统用于产生气泡气体的输,控制和获取最大压力数据,加热炉用于提供数据提取环境,升降系统用于控制气体输送及控制和加热炉内测量对象的相对位置,气氛控制系统用于保证加热炉的反应气氛,温度控制系统用于保证加热炉中的反应温度,控制显示系统用于对测量数据进行处理计算高温熔体表面张力并进行显示。该装置可以保证在良好的升温速率和精确的温度控制下快速精确的测量出高温熔体的表面张力。

The invention provides a device for measuring surface tension of high-temperature melt with the maximum bubble method, which includes a gas delivery and control system, a heating furnace, a lifting system, an atmosphere control system, a temperature control system and a control system. The gas delivery and control system is used for the delivery, control and acquisition of maximum pressure data of the gas that generates bubbles, the heating furnace is used to provide the data extraction environment, the lifting system is used to control the gas delivery and control the relative position of the measurement object in the heating furnace, and the atmosphere control The system is used to ensure the reaction atmosphere of the heating furnace, the temperature control system is used to ensure the reaction temperature in the heating furnace, and the control display system is used to process the measured data to calculate the surface tension of the high-temperature melt and display it. The device can ensure rapid and accurate measurement of the surface tension of the high-temperature melt under a good heating rate and precise temperature control.

Description

一种高温熔体最大气泡法测表面张力的装置A device for measuring surface tension by the maximum bubble method of high-temperature melt

技术领域technical field

本发明属于一种测量装置,具体涉及一种用最大气泡压力法测量高温熔体物性表面张力装置。The invention belongs to a measuring device, in particular to a device for measuring the surface tension of high-temperature melt physical properties by using the maximum bubble pressure method.

背景技术Background technique

高温熔体的表面张力是高温熔体的一种非常重要的参数,是影响多相体系传质和反应的关键因素之一。而对于冶金炉渣,特别是高钛渣,通过测量其表面张力,对泡沫化的原因和控制有重要的指导意义。The surface tension of high-temperature melt is a very important parameter of high-temperature melt, and it is one of the key factors affecting mass transfer and reaction of multi-phase system. For metallurgical slag, especially high-titanium slag, measuring its surface tension has important guiding significance for the cause and control of foaming.

目前测量高温熔体表面张力的测量方法主要有最大气泡压力法、拉筒法和静滴法等,其中拉筒法装置最简易,但无法满足测量精度上的要求。最大气泡压力法由Simon于1851年提出,后由Canter,Jaeger分别从理论和实用角度加以发展。实验的基本步骤是,将以毛细管插入待测液体内部,向管内缓慢通入惰性气体,随着吹入气体压力的增大,气泡逐渐长大,但气泡恰好是半球时,气泡内的压力达到最大值,此时通过测量气泡压力,计算得到液体的表面张力。但是,目前的测量装置中普遍存在无法满足测量精度和无法测量高温熔体的表面张力等缺点。At present, the measurement methods for measuring the surface tension of high-temperature melts mainly include the maximum bubble pressure method, the pulling method, and the static drop method. Among them, the pulling method is the simplest device, but it cannot meet the measurement accuracy requirements. The maximum bubble pressure method was proposed by Simon in 1851, and later developed by Canter and Jaeger from the theoretical and practical perspectives. The basic procedure of the experiment is to insert a capillary tube into the liquid to be tested, and slowly inject an inert gas into the tube. As the pressure of the blown gas increases, the bubbles grow gradually, but when the bubble is just hemisphere, the pressure inside the bubble reaches At this time, the surface tension of the liquid is calculated by measuring the bubble pressure. However, the current measuring devices generally have shortcomings such as the inability to meet the measurement accuracy and the inability to measure the surface tension of high-temperature melts.

发明内容Contents of the invention

针对现存的上述问题,本发明的目的是为解决上述问题而提供了一种可测量高温熔体表面张力,且测量精度高的测量装置。In view of the above existing problems, the purpose of the present invention is to provide a measuring device capable of measuring the surface tension of high-temperature melts with high measurement accuracy in order to solve the above problems.

为实现上述目的,本发明采用如下技术方案:一种高温熔体最大气泡法测表面张力的装置,包括气体输送及控制系统、加热炉、升降系统、气氛控制系统、温度控制系统和控制显示系统;In order to achieve the above object, the present invention adopts the following technical solutions: a device for measuring surface tension of high-temperature melt with the maximum bubble method, including gas delivery and control system, heating furnace, lifting system, atmosphere control system, temperature control system and control display system ;

气体输送及控制系统:包括第一惰性气体储存瓶、第一减压阀、数字式压 差计、毛细管安装装置和毛细管;Gas delivery and control system: including the first inert gas storage bottle, the first pressure reducing valve, digital differential pressure gauge, capillary installation device and capillary;

所述毛细管的上端通过毛细管安装装置固定,保证毛细管处于竖直状态;The upper end of the capillary is fixed by a capillary installation device to ensure that the capillary is in a vertical state;

所述第一惰性气体储存瓶的出气口通过气管与毛细管的上端连通,所述第一减压阀和数字式压差计分别设置在气管上,其中第一减压阀位于第一惰性气体储存瓶出气口侧;The gas outlet of the first inert gas storage bottle communicates with the upper end of the capillary through the gas pipe, and the first pressure reducing valve and the digital differential pressure gauge are respectively arranged on the gas pipe, wherein the first pressure reducing valve is located in the first inert gas storage bottle. The gas outlet side of the bottle;

加热炉:包括炉管、炉管围城的炉腔和位于炉腔外且用于给炉腔加热的硅钼加热体;Heating furnace: including the furnace tube, the furnace cavity surrounded by the furnace tube and the silicon-molybdenum heating body located outside the furnace cavity and used to heat the furnace cavity;

所述毛细管的底部通过插入炉管进入炉腔;The bottom of the capillary enters the furnace cavity by inserting the furnace tube;

升降系统:包括升降杆、光栅尺、光栅尺固定架、连接臂和升降杆驱动件;Lifting system: including lifting rod, grating ruler, grating ruler fixing frame, connecting arm and lifting rod drive;

所述连接臂的右端固定在升降杆的上部,所述毛细管安装装置固定在连接臂的左端;The right end of the connecting arm is fixed on the upper part of the lifting rod, and the capillary installation device is fixed on the left end of the connecting arm;

所述光栅尺用于检测连接臂上下移动的位移,其包括数据采集部和可在数据采集部上来回滑动的滑动部,所述滑动部与连接臂的右端固定连接,所述数据采集部固定在光栅尺固定架的顶端;The grating ruler is used to detect the displacement of the connecting arm moving up and down, and it includes a data acquisition part and a sliding part that can slide back and forth on the data collecting part. The sliding part is fixedly connected with the right end of the connecting arm, and the data collecting part is fixed At the top of the grating ruler holder;

所述升降杆驱动件用于驱动升降杆升降;The lifting rod driver is used to drive the lifting rod to go up and down;

气氛控制系统:包括第二惰性气体储存瓶、第二减压阀和导气管;Atmosphere control system: including the second inert gas storage bottle, the second pressure reducing valve and the gas guide tube;

所述导气管的一端与第二惰性气体储存瓶的出气口连通,另一端与加热炉的炉腔连通;One end of the gas guide pipe communicates with the gas outlet of the second inert gas storage bottle, and the other end communicates with the furnace cavity of the heating furnace;

所述第二减压阀设置在导气管上;The second decompression valve is arranged on the airway;

温度控制系统:包括热电偶和温控柜;Temperature control system: including thermocouple and temperature control cabinet;

所述热电偶的检测端设置加热炉的炉腔内,用于测量加热炉的炉腔内待测溶体的温度,热电偶的数据输出端与温控柜数据输入端连接,将所测温度信号输入温控柜,温控柜根据接收到的温度信号控制硅钼加热体的加热温度;The detecting end of the thermocouple is arranged in the furnace cavity of the heating furnace, and is used to measure the temperature of the melt to be measured in the furnace cavity of the heating furnace, and the data output terminal of the thermocouple is connected with the data input terminal of the temperature control cabinet, and the measured temperature signal Input the temperature control cabinet, and the temperature control cabinet controls the heating temperature of the silicon-molybdenum heating body according to the received temperature signal;

控制显示系统:包括控制器和显示设备;Control display system: including controller and display device;

所述数字式压差计的信号输出端与控制器的信号输入端连接,控制器的位 移控制信号输出端与升降杆驱动件连接,所述光栅尺的信号输出端与控制器的位移信号输入端连接,温控柜的温度信号输出端与控制器的温度信号输入端连接,温控柜的温度控制信号输入端与控制器的温度控制信号输出端连接;The signal output end of the digital differential pressure gauge is connected to the signal input end of the controller, the displacement control signal output end of the controller is connected to the lifting rod driver, and the signal output end of the grating ruler is connected to the displacement signal input end of the controller. The temperature signal output end of the temperature control cabinet is connected to the temperature signal input end of the controller, and the temperature control signal input end of the temperature control cabinet is connected to the temperature control signal output end of the controller;

所述控制器根据接收信号计算加热炉炉腔内待测熔体的表面张力;The controller calculates the surface tension of the melt to be measured in the furnace cavity of the heating furnace according to the received signal;

所述控制器的显示信号输出端与显示设备的显示信号输入端连接。The display signal output end of the controller is connected with the display signal input end of the display device.

作为优化,所述气体输送及控制系统还包括流量计;As an optimization, the gas delivery and control system also includes a flow meter;

所述流量计设置在气管上,且位于第一减压阀和数字式压差计之间。The flow meter is arranged on the gas pipe and is located between the first pressure reducing valve and the digital differential pressure meter.

作为优化,所述气体输送及控制系统还包括稳压计;As an optimization, the gas delivery and control system also includes a pressure regulator;

所述稳压计设置在气管上,且位于流量计和数字式压差计之间。The pressure stabilizing gauge is arranged on the gas pipe and is located between the flowmeter and the digital differential pressure gauge.

作为优化,所述气体输送及控制系统还包括针型阀;As an optimization, the gas delivery and control system also includes a needle valve;

所述针型阀设置在气管上,且位于稳压计和数字式压差计之间。The needle valve is arranged on the gas pipe, and is located between the pressure regulator and the digital differential pressure gauge.

作为优化,所述气体输送及控制系统还包括脱氧干燥瓶;As an optimization, the gas delivery and control system also includes a deoxygenation drying bottle;

所述脱氧干燥瓶设置在气管上,且位于针型阀和数字式压差计之间。The deoxygenation drying bottle is arranged on the gas pipe, and is located between the needle valve and the digital differential pressure gauge.

作为优化,所述控制器计算待测溶体表面张力的公式为:As an optimization, the formula for calculating the surface tension of the solution to be measured by the controller is:

σ=(P-ρgh)r/2 (2);σ=(P-ρ g h)r/2 (2);

其中,σ为待测熔体的表面张力,P为最大压力,r为毛细管的半径,ρ为待测熔体的密度,h为毛细管插入待测熔体的深度。Among them, σ is the surface tension of the melt to be measured, P is the maximum pressure, r is the radius of the capillary, ρ is the density of the melt to be measured, and h is the depth of the capillary inserted into the melt to be measured.

作为优化,所述流量计采用玻璃管浮子流量计。As an optimization, the flowmeter adopts a glass tube rotameter.

作为优化,所述稳压计为玻璃钢储气容器。As an optimization, the manometer is a glass fiber reinforced plastic gas storage container.

作为优化,所述数字式压差计采用型号为SYT2000J,测量范围为0-2000Pa,精度0.1Pa。As an optimization, the digital differential pressure gauge adopts a model of SYT2000J with a measuring range of 0-2000Pa and an accuracy of 0.1Pa.

作为优化,所述毛细管采用金属钽管,管内直径1.00mm。As an optimization, the capillary is a metal tantalum tube with an inner diameter of 1.00mm.

相对于现有技术,本发明具有如下优点:Compared with the prior art, the present invention has the following advantages:

1、采用硅钼加热体,最高工作温度可达长时间工作温度通过安装不同精度的热电偶能满足连续测试试样温度范围升温迅 速3h内炉温达到采用新进的PID控温系统,控温精度 1. Using silicon molybdenum heating body, the maximum working temperature can reach long time working temperature By installing thermocouples with different precision, it can meet the temperature range of continuous test samples The temperature rises rapidly within 3 hours and the furnace temperature reaches Using the latest PID temperature control system, the temperature control accuracy

2、采用数字式微压差计测量气泡最大压差,压力测量范围0~2000Pa,压差计精度0.1Pa,采用数字式光栅尺用于毛细管端口位置控制,控制精度±0.001mm;数字式的微压计和光栅尺避免了人为读数误差,重复性好,有效的提高了设备的测量精度。2. The maximum pressure difference of bubbles is measured by a digital micro-pressure differential meter. The pressure measurement range is 0-2000Pa, and the precision of the differential pressure meter is 0.1Pa. The digital grating ruler is used to control the position of the capillary port, and the control accuracy is ±0.001mm; Manometers and grating rulers avoid human reading errors, have good repeatability, and effectively improve the measurement accuracy of the equipment.

3、检测高温熔体物性的方法具备操作简单、数据可靠、测量过程可实时监测控制,可以较为广泛的用于高温熔体表面张力的测量和研究。3. The method for detecting the physical properties of high-temperature melt has simple operation, reliable data, real-time monitoring and control of the measurement process, and can be widely used in the measurement and research of the surface tension of high-temperature melt.

附图说明Description of drawings

图1为本发明高温熔体最大气泡法测表面张力的装置的结构示意图。Fig. 1 is a structural schematic diagram of the device for measuring surface tension by the maximum bubble method of high-temperature melt according to the present invention.

图1中的附图标记:第一惰性气体储存瓶1,第一减压阀2,流量计3,稳压计4,针型阀5,脱氧干燥瓶6,数字式压差计7,毛细管安装装置8,毛细管9,加热炉10,升降杆11,光栅尺12,升降杆驱动件13,第二惰性气体储存瓶14,第二减压阀15,导气管16,热电偶17,温控柜18,控制显示系统19。Reference signs in Fig. 1: first inert gas storage bottle 1, first pressure reducing valve 2, flow meter 3, pressure regulator 4, needle valve 5, deoxygenation drying bottle 6, digital differential pressure gauge 7, capillary Installation device 8, capillary tube 9, heating furnace 10, lifting rod 11, grating ruler 12, lifting rod drive member 13, second inert gas storage bottle 14, second pressure reducing valve 15, air guide tube 16, thermocouple 17, temperature control Cabinet 18, control display system 19.

具体实施方式detailed description

在本发明的描述中,需要理解的是,术语“上”、“下”、“左”、“右”“竖直”、“水平”、“顶”、“底”、“内”等指示的方位或位置关系为基于附图所示的方位或位置关系,仅是为了便于描述本发明和简化描述,而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本发明的限制。In describing the present invention, it is to be understood that the terms "upper", "lower", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", etc. indicate The orientation or positional relationship is based on the orientation or positional relationship shown in the drawings, and is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the referred device or element must have a specific orientation or be configured in a specific orientation. and operation, and therefore should not be construed as limiting the invention.

此外,术语“第一”、“第二”仅用于描述目的,而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。由此,限定有“第一”、“第二”的特征可以明示或者隐含地包括一个或者更多个该特征。In addition, the terms "first" and "second" are used for descriptive purposes only, and cannot be interpreted as indicating or implying relative importance or implicitly specifying the quantity of indicated technical features. Thus, a feature defined as "first" and "second" may explicitly or implicitly include one or more of these features.

一种高温熔体最大气泡法测表面张力的装置,包括气体输送及控制系统、加热炉、升降系统、气氛控制系统、温度控制系统和控制系统;A device for measuring the surface tension of a high-temperature melt with the maximum bubble method, including a gas delivery and control system, a heating furnace, a lifting system, an atmosphere control system, a temperature control system, and a control system;

气体输送及控制系统:包括第一惰性气体储存瓶1、第一减压阀2、数字式压差计7、毛细管安装装置8和毛细管9;Gas delivery and control system: including a first inert gas storage bottle 1, a first pressure reducing valve 2, a digital differential pressure gauge 7, a capillary installation device 8 and a capillary 9;

所述第一惰性气体储存瓶1的出气口通过气管与毛细管9连通,所述第一减压阀2和数字式压差计7分别设置在气管上,其中第一减压阀2位于第一惰性气体储存瓶1出气口侧;所述毛细管9的上端通过毛细管安装装置8固定,保证毛细管9处于竖直状态;The gas outlet of the first inert gas storage bottle 1 communicates with the capillary 9 through the gas pipe, and the first pressure reducing valve 2 and the digital differential pressure gauge 7 are respectively arranged on the gas pipe, wherein the first pressure reducing valve 2 is located at the first The gas outlet side of the inert gas storage bottle 1; the upper end of the capillary 9 is fixed by the capillary installation device 8 to ensure that the capillary 9 is in a vertical state;

具体实施时,第一惰性气体储存瓶1内装的惰性气体为氩气,氩气纯度大于99.9%。选择氩气的主要是因为氩气容易提纯工艺成熟,价格便宜能满足测量需要。另外氩气作为惰性气体既能保护发热体,也能保证在测量金属熔体时金属不会被氧化。During specific implementation, the inert gas contained in the first inert gas storage bottle 1 is argon, and the purity of argon is greater than 99.9%. The main reason for choosing argon is that argon is easy to purify and mature, and the price is cheap to meet the measurement needs. In addition, argon as an inert gas can not only protect the heating element, but also ensure that the metal will not be oxidized when measuring the metal melt.

作为优化,气体输送及控制系统还包括流量计3、稳压计4、针型阀5和脱氧干燥瓶6;所述流量计3设置在气管上,且位于第一减压阀2和数字式压差计7之间;所述稳压计4设置在气管上,且位于流量计3和数字式压差计7之间,所述稳压计4为玻璃钢储气容器;所述针型阀5设置在气管上,且位于稳压计4和数字式压差计7之间;所述脱氧干燥瓶6设置在气管上,且位于针型阀5和数字式压差计7之间。As an optimization, the gas delivery and control system also includes a flow meter 3, a pressure regulator 4, a needle valve 5 and a deoxygenation drying bottle 6; Between the differential pressure gauges 7; the pressure stabilizer 4 is arranged on the air pipe, and between the flowmeter 3 and the digital differential pressure gauge 7, the pressure stabilizer 4 is a glass fiber reinforced plastic gas storage container; the needle valve 5 is set on the trachea, and is located between the manometer 4 and the digital differential pressure gauge 7;

流量计1-3采用玻璃管浮子流量计,其设置主要是为了方便查看气管中气体流量,针型阀1-5是为了更加方便准确的调节和控制气管中的氩气,提高检测精度,因为在测量时需要保证气体从熔体中是间断冒出且速率在2秒左右1个气泡为宜。Flowmeters 1-3 use glass tube rotameters, which are mainly set for the convenience of viewing the gas flow in the gas pipe. Needle valves 1-5 are for more convenient and accurate adjustment and control of argon in the gas pipe, and improve detection accuracy, because When measuring, it is necessary to ensure that the gas emerges from the melt intermittently and the rate is about 1 bubble per second.

稳压计1-4为玻璃钢储气容器,其设置主要是起一个缓冲作用,进一步稳定气管中的压力,避免因为压力的突然增大对设备产生不利影响;The pressure regulator 1-4 is a glass fiber reinforced plastic gas storage container, and its setting is mainly to act as a buffer to further stabilize the pressure in the air pipe and avoid adverse effects on the equipment due to a sudden increase in pressure;

针型阀1-5的设置主要是为了更加精确的控制气管中气体的流速;The setting of needle valve 1-5 is mainly to control the flow rate of gas in the trachea more accurately;

脱氧干燥瓶1-6内装有脱氧和脱水剂用于对气管中的氩气进行脱氧和干燥,提高了装置的适用性和精确性,保证接触到熔体或熔渣的气体的纯度,减小对 熔体特别是金属液体的氧化而带来的误差;Deoxidation drying bottles 1-6 are equipped with deoxidation and dehydration agents to deoxidize and dry the argon in the gas pipe, which improves the applicability and accuracy of the device, ensures the purity of the gas contacting the melt or slag, and reduces the The error caused by the oxidation of the melt, especially the metal liquid;

所述数字式压差计1-7采用型号为SYT2000J,测量范围为0-2000Pa,精度0.1Pa。根据一直高温熔体的表面张力可以计算得到最大气泡法测得的压力差小于2000Pa,且数量级在1000Pa,故0-2000Pa的量程能满足绝大多数熔体表面张力的测量,另外精度0.1Pa更能保证结果的精确度;The digital differential pressure gauge 1-7 adopts the model SYT2000J, the measurement range is 0-2000Pa, and the precision is 0.1Pa. According to the surface tension of the high-temperature melt, it can be calculated that the pressure difference measured by the maximum bubble method is less than 2000Pa, and the order of magnitude is 1000Pa, so the range of 0-2000Pa can meet the measurement of the surface tension of most melts, and the accuracy is more than 0.1Pa. Can guarantee the accuracy of the results;

具体实施时,毛细管1-10采用金属钽管,对于氧化物熔体如高炉渣、电炉渣,其成分不会与金属钽发生反应且熔点高,故金属钽能满足测量要求。毛细管1-10管内直径1.00mm,由所测熔体的基本性质决定制成。In practice, the capillaries 1-10 use metal tantalum tubes. For oxide melts such as blast furnace slag and electric furnace slag, their components will not react with metal tantalum and have a high melting point, so metal tantalum can meet the measurement requirements. The inner diameter of capillary 1-10 is 1.00mm, which is determined by the basic properties of the measured melt.

具体实施时,所述气管上具有多个用于安装器件的螺纹孔,第一减压阀2流量计3、稳压计4和针型阀5分别通过螺纹连接的方式设置在气管上;During specific implementation, there are a plurality of threaded holes for installing devices on the air pipe, and the first pressure reducing valve 2, the flow meter 3, the pressure regulator 4 and the needle valve 5 are respectively arranged on the air pipe by threaded connection;

为了方便连接,脱氧干燥瓶6的进气口与针型阀5采用橡胶管连接,数字式压差计7、脱氧干燥瓶6和毛细管9通过三通管,三通管的第一个管口与脱氧干燥瓶6的出气口连通,三通管的第二个管口与数字式压差计7的检测端连通,三通管道的第三个管口与毛细管9的上端连通。In order to facilitate the connection, the air inlet of the deoxidation drying bottle 6 is connected with the needle valve 5 by a rubber tube, and the digital differential pressure gauge 7, the deoxygenation drying bottle 6 and the capillary tube 9 pass through a three-way pipe, and the first nozzle of the three-way pipe It communicates with the gas outlet of the deoxidizing drying bottle 6, the second nozzle of the three-way pipe communicates with the detection end of the digital differential pressure gauge 7, and the third nozzle of the three-way pipe communicates with the upper end of the capillary 9.

加热炉10:包括炉管、炉管围城的炉腔和位于炉腔外且用于给炉腔加热的硅钼加热体;所述毛细管9的底部通过插入炉管进入炉腔;Heating furnace 10: comprising a furnace tube, a furnace cavity surrounded by the furnace tube, and a silicon-molybdenum heating body located outside the furnace cavity and used to heat the furnace cavity; the bottom of the capillary 9 enters the furnace cavity by inserting the furnace tube;

所述具体实施时加热炉可以为硅钼炉,为本领域所通用的高温器件,只要符合测量熔体表面张力所需的参数条件,并无特殊要求。In the specific implementation, the heating furnace can be a silicon-molybdenum furnace, which is a high-temperature device commonly used in the field, and there is no special requirement as long as it meets the parameter conditions required for measuring the surface tension of the melt.

升降系统:包括升降杆11、光栅尺12、光栅尺固定架、连接臂和升降杆驱动件13;Lifting system: including lifting rod 11, grating ruler 12, grating ruler fixing frame, connecting arm and lifting rod driver 13;

所述升降杆11和光栅尺固定架竖直设置,且升降杆11和光栅尺固定架的底部分别固定在升降杆驱动件13的外壳上;The lifting rod 11 and the grating ruler fixing mount are vertically arranged, and the bottoms of the lifting rod 11 and the grating ruler fixing mount are respectively fixed on the shell of the lifting rod driver 13;

所述连接臂的右端固定在升降杆11的上部,所述毛细管安装装置8固定在连接臂的左端;The right end of the connecting arm is fixed on the top of the lifting rod 11, and the capillary installation device 8 is fixed on the left end of the connecting arm;

所述光栅尺12包括数据采集部和可在数据采集部上来回滑动的滑动部,所 述滑动部与连接臂的右端固定连接,所述数据采集部固定在光栅尺固定架的顶端;光栅尺12用于检测升降杆11上下移动的位移,光栅尺12最大量程520mm,精度为0.001mm,用于精确控制毛细管端与熔体液面的距离。Described grating ruler 12 comprises data acquisition part and the sliding part that can slide back and forth on data acquisition part, and described sliding part is fixedly connected with the right end of connecting arm, and described data acquisition part is fixed on the top of grating ruler fixed mount; 12 is used to detect the displacement of the lifting rod 11 moving up and down. The maximum range of the grating ruler 12 is 520mm, and the accuracy is 0.001mm, which is used to accurately control the distance between the end of the capillary and the liquid surface of the melt.

所述升降杆驱动件13用于驱动升降杆11升降。。The lifting rod driver 13 is used to drive the lifting rod 11 to go up and down. .

升降杆驱动件13驱动升降杆11升降,升降杆11带动与其固定连接的连接臂升降,从而固定在连接臂左端的毛细管9和光栅尺12的滑动部也随着连接臂升降,光栅尺12的数据采集部通过采集滑动部升降的位移,确定升降杆11升降的位移,从而最终确定毛细管9升降的位移。The lifting rod driver 13 drives the lifting rod 11 to rise and fall, and the lifting rod 11 drives the connecting arm fixedly connected with it to rise and fall, so that the capillary 9 and the sliding part of the grating ruler 12 fixed on the left end of the connecting arm also rise and fall along with the connecting arm, and the grating ruler 12 moves up and down. The data collection unit determines the lifting displacement of the lifting rod 11 by collecting the lifting displacement of the sliding part, so as to finally determine the lifting displacement of the capillary 9 .

气氛控制系统:包括第二惰性气体储存瓶14、第二减压阀15和导气管16;Atmosphere control system: including a second inert gas storage bottle 14, a second decompression valve 15 and an air guide tube 16;

所述导气管16的一端与第二惰性气体储存瓶14的出气口连通,另一端与加热炉的炉腔连通;所述第二减压阀15设置在导气管16上;One end of the gas guide pipe 16 communicates with the gas outlet of the second inert gas storage bottle 14, and the other end communicates with the furnace chamber of the heating furnace; the second pressure reducing valve 15 is arranged on the gas guide pipe 16;

具体实施时,第二减压阀15通过螺纹连接的方式设置在导气管16上,通过第二减压阀15的通断控制加热炉10炉内的气氛。During specific implementation, the second decompression valve 15 is provided on the gas guide pipe 16 through screw connection, and the atmosphere in the heating furnace 10 is controlled by the on-off of the second decompression valve 15 .

温度控制系统:包括热电偶17和温控柜18;Temperature control system: including thermocouple 17 and temperature control cabinet 18;

所述热电偶17的检测端设置加热炉的炉腔内,用于测量加热炉的炉腔内待测溶体的温度,热电偶17的数据输出端与温控柜18数据输入端连接;The detecting end of described thermocouple 17 is arranged in the furnace cavity of heating furnace, is used for measuring the temperature of the melt to be measured in the furnace cavity of heating furnace, and the data output end of thermocouple 17 is connected with temperature control cabinet 18 data input ends;

热电偶17将所测温度信号输入温控柜18,温控柜18根据接收到的温度信号控制加热炉10中通入硅钼加热体的电流大小,从而实现对加热炉10炉腔内温度的控制,将所测温度信号输入温控柜18,温控柜18根据接收到的温度信号控制硅钼加热体的加热温度;温控柜属于现有技术,其通过热电偶所测温度信号控制加热的加热温度也属于现有技术,不属于本发明的发明点,具体实施时可采用PID控制器。The thermocouple 17 inputs the measured temperature signal into the temperature control cabinet 18, and the temperature control cabinet 18 controls the current of the silicon-molybdenum heating body in the heating furnace 10 according to the received temperature signal, thereby realizing the temperature control of the furnace cavity of the heating furnace 10. Control, the measured temperature signal is input into the temperature control cabinet 18, and the temperature control cabinet 18 controls the heating temperature of the silicon-molybdenum heating body according to the received temperature signal; the temperature control cabinet belongs to the prior art, and it controls the heating through the temperature signal measured by the thermocouple The heating temperature also belongs to the prior art, and does not belong to the invention point of the present invention, and a PID controller can be used during specific implementation.

控制显示系统19:包括控制器和显示设备;Control display system 19: including a controller and a display device;

所述数字式压差计7的信号输出端与控制器的信号输入端连接,控制器的位移控制信号输出端与升降杆驱动件13连接,所述光栅尺12的信号输出端与 控制器的位移信号输入端连接,温控柜18的温度信号输出端与控制器的温度信号输入端连接,温控柜18的温度控制信号输入端与控制器的温度控制信号输出端连接;The signal output end of the digital differential pressure gauge 7 is connected to the signal input end of the controller, the displacement control signal output end of the controller is connected to the lifting rod driver 13, and the signal output end of the grating ruler 12 is connected to the controller's The displacement signal input terminal is connected, the temperature signal output terminal of the temperature control cabinet 18 is connected with the temperature signal input terminal of the controller, and the temperature control signal input terminal of the temperature control cabinet 18 is connected with the temperature control signal output terminal of the controller;

控制器通过控制升降杆驱动件13实现对升降杆11升降位移的精确控制,从而实现对毛细管9升降位移的精确控制。The controller realizes precise control of the lifting displacement of the lifting rod 11 by controlling the driving member 13 of the lifting rod, thereby realizing precise control of the lifting displacement of the capillary 9 .

所述控制器根据接收信号计算加热炉10炉腔内待测熔体的表面张力;The controller calculates the surface tension of the melt to be measured in the furnace cavity of the heating furnace 10 according to the received signal;

所述控制器的显示信号输出端与显示设备的显示信号输入端连接,显示设备用于显示温控柜18传输的炉腔内溶体的温度、升降杆11移动的位移、数字式压差计7测得的压差以及控制器计算的溶体表面张力。The display signal output end of the controller is connected to the display signal input end of the display device, and the display device is used to display the temperature of the melt in the furnace cavity transmitted by the temperature control cabinet 18, the displacement of the lifting rod 11, the digital differential pressure gauge 7 The measured differential pressure and the melt surface tension calculated by the controller.

所述控制器计算待测溶体表面张力的公式为:The formula for calculating the surface tension of the solution to be measured by the controller is:

最大气泡法原理公式为式(1);The principle formula of the maximum bubble method is formula (1);

进一步推导即可得到计算溶体表面张力的公式(2):The formula (2) for calculating the surface tension of the solution can be obtained by further derivation:

σ=(P-ρgh)r/2 (2);σ=(P-ρ g h)r/2 (2);

其中,σ为待测熔体的表面张力,P为最大压力,r为毛细管的半径,ρ为待测熔体的密度,h为毛细管9插入待测熔体的深度。Wherein, σ is the surface tension of the melt to be measured, P is the maximum pressure, r is the radius of the capillary, ρ is the density of the melt to be measured, and h is the depth at which the capillary 9 is inserted into the melt to be measured.

应用上述高温熔体最大气泡法测表面张力的装置测量熔体表面张力的具体步骤如下:The specific steps for measuring the surface tension of the melt by using the above-mentioned device for measuring the surface tension of the high-temperature melt maximum bubble method are as follows:

以下所举的高炉渣为熔体熔渣,但是完全可以用于其他熔体熔渣:The blast furnace slags listed below are molten slags, but can be used for other molten slags:

S1:加热炉采用硅钼加热炉,硅钼炉的炉腔内放入坩埚,硅钼加热体采用硅钼棒,采用硅钼棒对坩埚内的熔渣进行加热,直至炉渣熔化,保温2个小时使炉渣成分均匀;S1: The heating furnace adopts silicon-molybdenum heating furnace, and the crucible is placed in the furnace cavity of the silicon-molybdenum furnace. The silicon-molybdenum heating body uses silicon-molybdenum rods, and the silicon-molybdenum rods are used to heat the slag in the crucible until the slag melts. hour to make the composition of slag uniform;

S2:启动升降系统,升降杆驱动件13驱动升降杆11移动,使毛细管9的下端正好位于坩埚内熔渣表面上方,且与熔渣表面不接触,此时将数字式压差计7的压差计调零;升降杆驱动件13驱动升降杆11移动,使毛细管9的下端 下降至恰好与炉渣表面接触,此时控制器控制升降杆驱动件13驱动升降杆11移动,使升降杆11的初始位置归零;S2: Start the lifting system, the lifting rod driver 13 drives the lifting rod 11 to move, so that the lower end of the capillary 9 is just above the slag surface in the crucible, and does not contact the slag surface. The difference meter is zeroed; the lifting rod driving part 13 drives the lifting rod 11 to move, so that the lower end of the capillary 9 falls to just contact with the slag surface, and at this time, the controller controls the lifting rod driving part 13 to drive the lifting rod 11 to move, so that the lifting rod 11 Return the initial position to zero;

S3:打开第一减压阀2,通过第一减压阀2和针型阀控制氩气气体流量,此时数字式压差计7出现数值,当炉渣内部能够稳定、缓慢的产生气泡时,数字式压差计7的数值由小到大变化,升降杆驱动件13驱动升降杆11移动,从而带动毛细管9移动,改变毛细管9的插入炉渣的深度,得到各个深度下的最大压差,毛细管9插入炉渣的深度分别记为h1,h2,h3,毛细管9插入炉渣的各个深度下对应的最大压差分别记为P1,P2,P3S3: Open the first pressure reducing valve 2, and control the flow of argon gas through the first pressure reducing valve 2 and the needle valve. At this time, the digital differential pressure gauge 7 shows a value. When bubbles can be stably and slowly generated inside the slag, The value of the digital differential pressure gauge 7 changes from small to large. The lifting rod driver 13 drives the lifting rod 11 to move, thereby driving the capillary 9 to move, changing the depth of the capillary 9 inserted into the slag, and obtaining the maximum pressure difference at each depth. 9 The depths inserted into the slag are denoted as h 1 , h 2 , h 3 respectively, and the maximum pressure differences corresponding to the respective depths of the capillary 9 inserted into the slag are denoted as P 1 , P 2 , P 3 ;

S4:根据公式,用P1,P2和h1,h2可以计算得到ρg的值,即:P2-P1=ρg(h2-h1),再根据P3和h3以及计算得到的ρg代入公式(2)便可得到熔渣的表面张力。S4: According to the formula, use P 1 , P 2 and h 1 , h 2 to calculate the value of ρ g , namely: P 2 -P 1 = ρ g (h 2 -h 1 ), and then according to P 3 and h 3 And the calculated ρ g is substituted into the formula (2) to obtain the surface tension of the slag.

S5:测试完成后,升起毛细管9,关闭升温系统,待加热炉体冷却到室温后清洗炉体清洁设备。S5: After the test is completed, raise the capillary 9, close the heating system, and clean the furnace body cleaning equipment after the heating furnace body cools down to room temperature.

该装置实现了快速测量的目的,而且精度和自动化程度高,可以很好的满足实验室和工业上的测量要求。The device achieves the purpose of rapid measurement, and has high precision and automation, which can well meet the measurement requirements of laboratories and industries.

最后所应说明的是,以上实施例仅用以说明本发明的技术方案而非限制,尽管参照较佳实施例对本发明进行了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,其均应涵盖在本发明的权利要求范围当中。Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention without limitation. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be Modifications or equivalent replacements of the technical solutions without departing from the spirit and scope of the technical solutions of the present invention shall be covered by the scope of the claims of the present invention.

Claims (10)

1.一种高温熔体最大气泡法测表面张力的装置,其特征在于:包括气体输送及控制系统、加热炉、升降系统、气氛控制系统、温度控制系统和控制显示系统;1. A device for measuring surface tension by the maximum bubble method of high-temperature melt, characterized in that: it includes a gas delivery and control system, a heating furnace, a lifting system, an atmosphere control system, a temperature control system and a control display system; 气体输送及控制系统:包括第一惰性气体储存瓶(1)、第一减压阀(2)、数字式压差计(7)、毛细管安装装置(8)和毛细管(9);Gas delivery and control system: including a first inert gas storage bottle (1), a first pressure reducing valve (2), a digital differential pressure gauge (7), a capillary installation device (8) and a capillary (9); 所述毛细管(9)的上端通过毛细管安装装置(8)固定,保证毛细管(9)处于竖直状态;The upper end of the capillary (9) is fixed by the capillary mounting device (8), ensuring that the capillary (9) is in a vertical state; 所述第一惰性气体储存瓶(1)的出气口通过气管与毛细管(9)的上端连通,所述第一减压阀(2)和数字式压差计(7)分别设置在气管上,其中第一减压阀(2)位于第一惰性气体储存瓶(1)出气口侧;The gas outlet of the first inert gas storage bottle (1) communicates with the upper end of the capillary (9) through the gas pipe, and the first pressure reducing valve (2) and the digital differential pressure gauge (7) are respectively arranged on the gas pipe, Wherein the first decompression valve (2) is located at the gas outlet side of the first inert gas storage bottle (1); 加热炉(10):包括炉管、炉管围城的炉腔和位于炉腔外且用于给炉腔加热的硅钼加热体;Heating furnace (10): including the furnace tube, the furnace cavity surrounded by the furnace tube and the silicon-molybdenum heating body located outside the furnace cavity and used to heat the furnace cavity; 所述毛细管(9)的底部通过插入炉管进入炉腔;The bottom of the capillary (9) enters the furnace cavity by inserting the furnace tube; 升降系统:包括升降杆(11)、光栅尺(12)、光栅尺固定架、连接臂和升降杆驱动件(13);Lifting system: including lifting rod (11), grating ruler (12), grating ruler fixing frame, connecting arm and lifting rod driving member (13); 所述连接臂的右端固定在升降杆(11)的上部,所述毛细管安装装置(8)固定在连接臂的左端;The right end of the connecting arm is fixed on the top of the elevating rod (11), and the capillary installation device (8) is fixed on the left end of the connecting arm; 所述光栅尺(12)用于检测连接臂上下移动的位移,其包括数据采集部和可在数据采集部上来回滑动的滑动部,所述滑动部与连接臂的右端固定连接,所述数据采集部固定在光栅尺固定架的顶端;The grating ruler (12) is used to detect the displacement of the connecting arm moving up and down, and it includes a data acquisition part and a sliding part that can slide back and forth on the data collecting part, and the sliding part is fixedly connected with the right end of the connecting arm. The acquisition part is fixed on the top of the grating ruler fixing frame; 所述升降杆驱动件(13)用于驱动升降杆(11)升降;The lifting rod driver (13) is used to drive the lifting rod (11) to lift; 气氛控制系统:包括第二惰性气体储存瓶(14)、第二减压阀(15)和导气管(16);Atmosphere control system: comprising a second inert gas storage bottle (14), a second decompression valve (15) and an air guide tube (16); 所述导气管(16)的一端与第二惰性气体储存瓶(14)的出气口连通,另一端与加热炉的炉腔连通;One end of the gas guide pipe (16) communicates with the gas outlet of the second inert gas storage bottle (14), and the other end communicates with the furnace chamber of the heating furnace; 所述第二减压阀(15)设置在导气管(16)上;The second decompression valve (15) is arranged on the airway (16); 温度控制系统:包括热电偶(17)和温控柜(18);Temperature control system: including thermocouple (17) and temperature control cabinet (18); 所述热电偶(17)的检测端设置加热炉的炉腔内,用于测量加热炉的炉腔内待测溶体的温度,热电偶(17)的数据输出端与温控柜(18)数据输入端连接,将所测温度信号输入温控柜(18),温控柜(18)根据接收到的温度信号控制硅钼加热体的加热温度;The detecting end of described thermocouple (17) is arranged in the furnace cavity of heating furnace, is used for measuring the temperature of the melt to be measured in the furnace cavity of heating furnace, and the data output terminal of thermocouple (17) and temperature control cabinet (18) data The input end is connected, and the measured temperature signal is input into the temperature control cabinet (18), and the temperature control cabinet (18) controls the heating temperature of the silicon-molybdenum heating body according to the received temperature signal; 控制显示系统(19):包括控制器和显示设备;Control display system (19): including a controller and a display device; 所述数字式压差计(7)的信号输出端与控制器的信号输入端连接,控制器的位移控制信号输出端与升降杆驱动件(13)连接,所述光栅尺(12)的信号输出端与控制器的位移信号输入端连接,温控柜(18)的温度信号输出端与控制器的温度信号输入端连接,温控柜(18)的温度控制信号输入端与控制器的温度控制信号输出端连接;The signal output end of the digital differential pressure gauge (7) is connected with the signal input end of the controller, the displacement control signal output end of the controller is connected with the lifting rod driver (13), and the signal of the grating ruler (12) The output end is connected with the displacement signal input end of the controller, the temperature signal output end of the temperature control cabinet (18) is connected with the temperature signal input end of the controller, and the temperature control signal input end of the temperature control cabinet (18) is connected with the temperature of the controller. Control signal output terminal connection; 所述控制器根据接收信号计算加热炉(10)炉腔内待测熔体的表面张力;The controller calculates the surface tension of the melt to be measured in the furnace cavity of the heating furnace (10) according to the received signal; 所述控制器的显示信号输出端与显示设备的显示信号输入端连接。The display signal output end of the controller is connected with the display signal input end of the display device. 2.如权利要求1所述的高温熔体最大气泡法测表面张力的装置,其特征在于:所述气体输送及控制系统还包括流量计(3);2. The device for measuring surface tension by the maximum bubble method of high-temperature melt as claimed in claim 1, characterized in that: the gas delivery and control system also includes a flow meter (3); 所述流量计(3)设置在气管上,且位于第一减压阀(2)和数字式压差计(7)之间。The flow meter (3) is arranged on the gas pipe, and is located between the first pressure reducing valve (2) and the digital differential pressure meter (7). 3.如权利要求2所述的高温熔体最大气泡法测表面张力的装置,其特征在于:所述气体输送及控制系统还包括稳压计(4);3. The device for measuring the surface tension of the high-temperature melt maximum bubble method as claimed in claim 2, characterized in that: the gas delivery and control system also includes a manometer (4); 所述稳压计(4)设置在气管上,且位于流量计(3)和数字式压差计(7)之间。The pressure stabilizing meter (4) is arranged on the gas pipe, and is located between the flow meter (3) and the digital differential pressure meter (7). 4.如权利要求3所述的高温熔体最大气泡法测表面张力的装置,其特征在于:所述气体输送及控制系统还包括针型阀(5);4. The device for measuring surface tension by the maximum bubble method of high-temperature melt as claimed in claim 3, characterized in that: the gas delivery and control system also includes a needle valve (5); 所述针型阀(5)设置在气管上,且位于稳压计(4)和数字式压差计(7)之间。The needle valve (5) is arranged on the gas pipe, and is located between the pressure regulator (4) and the digital differential pressure gauge (7). 5.如权利要求4所述的高温熔体最大气泡法测表面张力的装置,其特征在于:所述气体输送及控制系统还包括脱氧干燥瓶(6);5. the device of measuring surface tension by the maximum bubble method of high-temperature melt as claimed in claim 4, is characterized in that: said gas delivery and control system also includes a deoxidizing drying bottle (6); 所述脱氧干燥瓶(6)设置在气管上,且位于针型阀(5)和数字式压差计(7)之间。The deoxygenation drying bottle (6) is arranged on the gas pipe, and is located between the needle valve (5) and the digital differential pressure gauge (7). 6.如权利要求1-5任一项所述的高温熔体最大气泡法测表面张力的装置,其特征在于:所述控制器计算待测溶体表面张力的公式为:6. The device for measuring surface tension by the maximum bubble method of high-temperature melt as claimed in any one of claims 1-5, wherein the formula for calculating the surface tension of the melt to be measured by the controller is: σ=(P-ρgh)r/2 (2);σ=(P-ρ g h)r/2 (2); 其中,σ为待测熔体的表面张力,P为最大压力,r为毛细管的半径,ρ为待测熔体的密度,h为毛细管(9)插入待测熔体的深度。Wherein, σ is the surface tension of the melt to be measured, P is the maximum pressure, r is the radius of the capillary, ρ is the density of the melt to be measured, and h is the depth at which the capillary (9) is inserted into the melt to be measured. 7.如权利要求6所述的高温熔体最大气泡法测表面张力的装置,其特征在于:所述流量计(3)采用玻璃管浮子流量计。7. The device for measuring surface tension of high-temperature melt with the maximum bubble method according to claim 6, characterized in that: said flowmeter (3) adopts a glass tube float flowmeter. 8.如权利要求2所述的高温熔体最大气泡法测表面张力的装置,其特征在于:所述稳压计(4)为玻璃钢储气容器。8. The device for measuring surface tension of high-temperature melt with the maximum bubble method according to claim 2, characterized in that: the pressure stabilizer (4) is a glass fiber reinforced plastic gas storage container. 9.如权利要求6所述的高温熔体最大气泡法测表面张力的装置,其特征在于:所述数字式压差计(7)采用型号为SYT2000J,测量范围为0-2000Pa,精度0.1Pa。9. The device for measuring surface tension by the maximum bubble method of high-temperature melt as claimed in claim 6, characterized in that: the digital differential pressure meter (7) adopts a model of SYT2000J, a measurement range of 0-2000Pa, and an accuracy of 0.1Pa . 10.如权利要求1所述的高温熔体最大气泡法测表面张力的装置,其特征在于:所述毛细管(9)采用金属钽管,管内直径1.00mm。10. The device for measuring surface tension of high-temperature melt with the maximum bubble method according to claim 1, characterized in that: the capillary (9) is a metal tantalum tube with an inner diameter of 1.00mm.
CN201610655866.5A 2016-08-11 2016-08-11 Device for measuring surface tension by using high-temperature melt maximum bubble method Pending CN106442228A (en)

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