CN103411854A - Interface tension measuring device and method by hanging drop or bubble blowing way under high pressure - Google Patents

Interface tension measuring device and method by hanging drop or bubble blowing way under high pressure Download PDF

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Publication number
CN103411854A
CN103411854A CN2013103206872A CN201310320687A CN103411854A CN 103411854 A CN103411854 A CN 103411854A CN 2013103206872 A CN2013103206872 A CN 2013103206872A CN 201310320687 A CN201310320687 A CN 201310320687A CN 103411854 A CN103411854 A CN 103411854A
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China
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pressure chamber
pressure
liquid
tubule
gas
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CN2013103206872A
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Chinese (zh)
Inventor
刘瑜
宋永臣
蒋兰兰
赵越超
杨明军
赵佳飞
张毅
王大勇
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大连理工大学
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Priority to CN2013103206872A priority Critical patent/CN103411854A/en
Publication of CN103411854A publication Critical patent/CN103411854A/en

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Abstract

The invention relates to an interface tension measuring device and method by a hanging drop or bubble blowing way under high pressure and belongs to the technical field of high-temperature high-pressure interface tension measuring. The device comprises a window pressure chamber device composed of a metal pressure chamber cylinder body and high pressure resistant glasses at two ends, a liquid drop/bubble injection device, a support and locking device and a photo and data processing device, wherein a liquid/gas inlet hole is formed in the side wall of the pressure chamber cylinder body and connected with a gas cylinder or a liquid charging pump through a quick connector, so as to realize the feeding of environmental gas or liquid into the pressure chamber cylinder body; a liquid/gas outlet hole is connected with a three-way connector, one path of the three-way connector is connected with a drain valve, and the other path is connected with a vacuum pump for vacuum-pumping of the pressure chamber; the liquid drop/bubble injection device comprises an injection tube and a pressure sensor; the injection tube is inserted into the cylinder body, and is sealed and connected with the pressure sensor to monitor the injection pressure, and the other end of the injection tube is connected with the liquid charging pump or the gas cylinder through a precision needle valve; the support and locking device comprises a base, a support frame and a locking bolt; the photo and data processing device comprises a CCD camera, a backlight and a data processing computer.

Description

Hanging drop or Bubbling method interfacial tension measurement mechanism and measuring method under a kind of high pressure
Technical field
The invention belongs to surface and interface tonometry technical field, relate to a kind of measurement mechanism and measuring method that under high pressure adopts hanging drop or Bubbling method to measure interfacial tension between oil gentle (nitrogen, carbon dioxide, gaseous hydrocarbon etc.).
Background technology
Adopting the gas displacement crude oil such as nitrogen, carbon dioxide, gaseous hydrocarbon is the effective means that improves oil recovery (Enhanced Oil Recovery, EOR).Interfacial tension between injection process Crude Oil and gas is that crude oil flows and one of the important control parameter of redistribution in stratum, is also the key factor that affects efficiency of displacement.Therefore, before carrying out actual displacement engineering project, must carry out Measurement accuracy to the interfacial tension between crude oil and displacement gas, and by a large amount of analysis of experimental data, affect the principal element of interfacial tension, thereby select the more reasonably technical parameters such as injection pressure, injection rate.
Interfacial tension experiments of measuring method between the oil-gas two-phase mainly comprises: 1) capillary rise method, 2) sessile drop method, 3) hang sheet method, 4) rotation drips a method, 5) sessile drop method etc.Wherein most widely used is rear three kinds of methods.The principle of hanging the measurement of sheet method is to utilize the balance of interfacial tension and pulling force, adopts the method for direct dynamometry to measure, and is applicable to the measurement of interfacial tension between the little two-phase fluid of density difference; The rotation method of dripping is that two-phase fluid is put into to the rotation of horizontal tube high speed, utilizes the balance of centrifugal force and interfacial tension indirectly to measure, and the method requires two to be on good terms and obviously to distinguish and higher density is transparent mutually.Above-mentioned two kinds of method ratios are more suitable for the liquid-liquid two-phase interface tonometry, measure significant limitation is arranged for gas-liquid two-phase.
Sessile drop method is best suited for the method that interfacial tension is measured between gas-liquid two-phase.The method is that the larger liquid of the density tubule that communicated is expelled in environmental gas, under the effect of interfacial tension and gravity, form effigurate drop, by the photo-optics method, measure the form parameter of drop, the density difference that is aided with two-phase fluid just can calculate interfacial tension.For the situation that is difficult to form drop, can adopt in liquid and blast gas, under the effect of interfacial tension and buoyancy, form bubble, photograph is identical with sessile drop method with computing method.The photo-optics system of hanging drop or Bubbling method measurement interfacial tension is very ripe at present, and relevant supporting image processing and software for calculation are also very perfect, can obtain very accurately the interfacial tension of gas-liquid two-phase.Yet test at present great majority, be all to carry out under normal temperature, normal pressure, under high pressure and variable temperature condition, also need to have withstand voltage except optical system and with the pressure vessel of transparent window, therefore experiment has very large difficulty.The present invention is exactly the device for interfacial tension measurement under high pressure of developing in order to address this problem, this device can be applied to sessile drop method and two kinds of interfacial tension measuring methods of Bubbling method, can between two kinds of methods, arbitrarily switch, simple to operate, coordinate the optical photographing system can the Measurement accuracy high pressure under interfacial tension between gas-liquid two-phase.
Summary of the invention
The invention provides hanging drop or Bubbling method interfacial tension measurement mechanism and measuring method under a kind of high pressure, solution, can't be high pressure resistant, control temperature and two kinds of measuring methods and the problem such as can not switch fast when adopting sessile drop method or Bubbling method to measure the gas-liquid two-phase interfacial tension.
Hanging drop or Bubbling method interfacial tension measurement mechanism under a kind of high pressure, comprise visual reactor, injection device, support and locking device, take pictures and data processing equipment, visual reactor comprises metal form pressure chamber (11), gas-liquid joint A(12), gas-liquid joint B(13), bleed valve (14), heating tape and muff (15), temperature probe (16); Metal form pressure chamber is cylindrical barrel, comprise pressure chamber's cylindrical shell (111) and high pressure resistant glass (112), pressure chamber's cylindrical shell (111) two ends have draw-in groove to put into circular high pressure resistant glass (112), fixing and sealing between the two, push down circular high pressure resistant glass (112) but end cap on have circular port to make the two ends transmitted light; On pressure chamber's cylindrical shell (111) sidewall, have two manhole appendixs that become 90 °; With gas-liquid joint A(12) connection manhole appendix A(117) with gas cylinder or liquid charge pump, inject environmental gas or liquid in pressure chamber's cylindrical shell, with gas-liquid joint B(13) connection manhole appendix B(118) and threeway, a road connection bleed valve (14) of threeway; Another road connects vacuum pump, pressure chamber's cylinder body outer wall parcel heating tape and muff (15), and pressure chamber's cylinder body bottom inserts temperature probe (16);
Injection device comprises injection tubule (21), pressure transducer (22), pressure chamber's cylinder lateral wall has between two manhole appendixs wears the wall pore, to inject tubule (21) is inserted in pressure chamber from wear the wall pore, for injecting fluid or gas, form drop or bubble, the external diameter of injection tubule can be in 0.5 to 2.0mm scope, the injection tubule inserts the degree of depth free adjustment of pressure chamber, the injection tubule is inserted in cylindrical shell and seals with pressure chamber's cylindrical shell, injection tubule other end connecting tee, one end of threeway connects liquid charge pump or gas cylinder, other end Bonding pressure sensor (22) monitoring injection pressure,
Support and locking device comprise base (311), bracing frame (312) and clamping screw (313), and visual reactor rotates on bracing frame, and uses the clamping screw fixed position, will inject after tubule is turned to the bottom, pressure chamber and carry out the Bubbling method measurement;
Take pictures and data processing equipment, comprise CCD camera (41), backlight (42) and data handling machine (43).
Said apparatus carries out the measuring method of interfacial tension measurement, comprises the following steps:
Injection tubule position is adjusted: unclamp and can regulate cutting ferrule, regulate the degree of depth of injection tubule (21) insertion pressure chamber's cylindrical shell (111), open backlight (42) and CCD camera (41), by CCD, observe the form center that the exit end face that makes tubule is in the CCD camera, locking can be regulated cutting ferrule;
Experimental technique switching: according to adopting hanging drop or Bubbling method to measure, supporting and the upper rotating metallic form pressure chamber (11) of locking device (31), while adopting sessile drop method, will inject tubule (21) rotation to top and surface level upright position, while adopting Bubbling method, will inject tubule (21) rotation to below and surface level upright position, and with clamping screw (313), that metal form pressure chamber (11) is fixing;
Form hyperbaric environment: close bleed valve (14), with vacuum pump, pressure chamber is vacuumized, open the valve of gas cylinder or liquid charge pump, to being filled with environmental gas in pressure chamber or liquid reaches experimental pressure, open heating tape and muff (15) to environmental gas or heating liquid to experimental temperature;
Injecting step, with liquid charge pump or gas cylinder, inject drop or bubble by the adjustment precision needle-valve, by injection tubule (21), in environmental gas or liquid, form sizeable hanging drop or bubble, have retaining valve to prevent environmental gas or liquid backflow between injection tubule (21) and needle-valve;
Take pictures and calculate: shape, the size of by CCD camera (41), observing drop or bubble, according to injection tubule (21) outside dimension, the scale parameter of taking pictures of CCD camera (41) is set, take the still photo of drop or bubble, calculate the physical size parameter of drop or bubble, the density difference that is aided with gas-liquid two-phase calculates interfacial tension.
Effect of the present invention and benefit are that under a kind of high pressure, hanging drop or Bubbling method interfacial tension measurement mechanism can adopt sessile drop method or two kinds of methods of Bubbling method to carry out the liquid-gas interface tonometry, and can between two kinds of methods, arbitrarily switch, easy and simple to handle, its working temperature, pressure are controllable and measurable, can realize the Measurement accuracy of gas-liquid two-phase interfacial tension under High Temperature High Pressure.
The accompanying drawing explanation
Fig. 1 is applicating flow chart of the present invention.
Fig. 2 (a) is the structural drawing of form pressure chamber device in the present invention.
Fig. 2 (b) is the side view of form pressure chamber device in the present invention.
In figure: 11-metal form pressure chamber, 12-gas-liquid joint A, 13-gas-liquid joint B, the 14-bleed valve, 15-heating tape and muff, 16-temperature probe, 21-injects tubule, the 22-pressure transducer, and 31-supports and locking device, the 41-CCD camera, the 42-backlight, 43-data handling machine, 111-pressure chamber cylindrical shell, the high pressure resistant glass of 112-, 113-pressure end cap, back-up ring and O-ring seal before 114-set collar, 115-, back-up ring after 116-, 117-manhole appendix A, 118-manhole appendix B, 311-base, the 312-bracing frame, the 313-clamping screw.
Embodiment
Below in conjunction with technical scheme and accompanying drawing, describe the specific embodiment of the present invention in detail.
The sessile drop method of take is measured interfacial tension and is example, in conjunction with Fig. 1, Fig. 2 (a), Fig. 2 (b), further sets forth the course of work of the present invention and is:
After being placed on metal form pressure chamber 11 on bracing frame 312, adjust its position, make to inject tubule 21 and be in perpendicular to the surface level position, then screw clamping screw 313.Regulate the degree of depth of injection tubule 21 insertion metal form pressure chambers 11, open the software of taking pictures on backlight 42 turn-on data process computer 43, by CCD camera 41, observe, with regulating cutting ferrule locking, inject tubule 21 when the exit end face of injecting tubule 21 is in the form center of CCD camera 41.By gas-liquid joint A12 connection metal form pressure chamber 11 and gas cylinder, by gas-liquid joint B13 and threeway connection metal form pressure chamber 11, bleed valve 14 and vacuum pump, connect injection tubule 21, liquid charge pump and pressure transducer 22 by threeway.
Close bleed valve 14 and gas cylinder, liquid charge pump valve, open the vacuum pump valve and metal form pressure chamber 11 is vacuumized.After vacuum tightness reaches requirement, close the vacuum pump valve, open gas cylinder valve and meet the requirements of pressure to the interior injection environmental gas of metal form pressure chamber 11.
With the environmental gas heating in heating tape and 15 pairs of metal form pressure chambers of muff 11, reach experimental temperature.
With liquid charge pump, to the interior injection drop of metal form pressure chamber 11, reach the suitable injection that stops when big or small by CCD camera 41 observed drop.
Regulate the suitable brightness of backlight 42, the drop image obtained by CCD camera 41 is presented on data handling machine 43, presses shutter and takes pictures.
Runs image processing and analysis software on computing machine 43, calculate interfacial tension.
While adopting Bubbling method to measure interfacial tension, first clamping screw 313 is unclamped, by metal form pressure chamber 11 Rotate 180 ° on bracing frame 312, make to inject bottom and the surface level upright position that tubule 21 forwards metal form pressure chamber 11 to, then clamping screw 313 is tightened.Gas cylinder and liquid charge pump during said process is described exchange, and the environmental gas of injection becomes environmental liquids, and drop becomes bubble, and other operation stepss are identical.

Claims (5)

1. hanging drop or Bubbling method interfacial tension measurement mechanism under a high pressure, comprise visual reactor, injection device, support and locking device, take pictures and data processing equipment, it is characterized in that,
Visual reactor comprises metal form pressure chamber (11), gas-liquid joint A(12), gas-liquid joint B(13), bleed valve (14), heating tape and muff (15) and temperature probe (16); Metal form pressure chamber is cylindrical barrel, comprise pressure chamber's cylindrical shell (111) and high pressure resistant glass (112), pressure chamber's cylindrical shell (111) two ends have draw-in groove to put into circular high pressure resistant glass (112), fixing and sealing between the two, push down circular high pressure resistant glass (112) but end cap on have circular port to make the two ends transmitted light; On pressure chamber's cylindrical shell (111) sidewall, have two manhole appendixs that become 90 °; With gas-liquid joint A(12) connection manhole appendix A(117) with gas cylinder or liquid charge pump, inject environmental gas or liquid in pressure chamber's cylindrical shell, with gas-liquid joint B(13) connection manhole appendix B(118) and threeway, a road connection bleed valve (14) of threeway; Another road connects vacuum pump, pressure chamber's cylinder body outer wall parcel heating tape and muff (15), and pressure chamber's cylinder body bottom inserts temperature probe (16);
Injection device comprises injection tubule (21), pressure transducer (22), pressure chamber's cylinder lateral wall has between two manhole appendixs wears the wall pore, to inject tubule (21) is inserted in pressure chamber from wear the wall pore, for injecting fluid or gas, form drop or bubble, the external diameter of injection tubule is in 0.5 to 2.0mm scope, the injection tubule inserts the degree of depth free adjustment of pressure chamber, the injection tubule is inserted in cylindrical shell and seals with pressure chamber's cylindrical shell, injection tubule other end connecting tee, one end of threeway connects liquid charge pump or gas cylinder, other end Bonding pressure sensor (22) monitoring injection pressure,
Support and locking device comprise base (311), bracing frame (312) and clamping screw (313), and visual reactor rotates on bracing frame, and uses the clamping screw fixed position, will inject after tubule is turned to the bottom, pressure chamber and carry out the Bubbling method measurement;
Take pictures and data processing equipment, comprise CCD camera (41), backlight (42) and data handling machine (43).
2. hanging drop or Bubbling method interfacial tension measurement mechanism under high pressure as claimed in claim 1, it is characterized in that: described injection tubule (21) is the stainless-steel tube of 2mm or 1.6mm external diameter, and the sealing means adopted with pressure chamber's cylindrical shell (111) seals for regulating cutting ferrule.
3. hanging drop or Bubbling method interfacial tension measurement mechanism under high pressure as claimed in claim 1 or 2, it is characterized in that: described high pressure resistant glass (112) is greater than the high printing opacity quartz glass of 15mm for thickness.
4. the method that under the described high pressure of claim 1 or 2, hanging drop or Bubbling method interfacial tension measurement mechanism carry out the interfacial tension measurement is characterized in that comprising the following steps:
Injection tubule position set-up procedure, unclamp and can regulate cutting ferrule, regulate the degree of depth of injection tubule (21) insertion pressure chamber's cylindrical shell (111), open backlight (42) and CCD camera (41), by CCD, observe the form center that the exit end face that makes tubule is in the CCD camera, locking can be regulated cutting ferrule;
The experimental technique switch step, according to adopting hanging drop or Bubbling method, measure, supporting and the upper rotating metallic form pressure chamber (11) of locking device (31), while adopting sessile drop method, will inject tubule (21) rotation to top and surface level upright position, while adopting Bubbling method, will inject tubule (21) rotation to below and surface level upright position, and with clamping screw (313), that metal form pressure chamber (11) is fixing;
Form the hyperbaric environment step, close bleed valve (14), with vacuum pump, pressure chamber is vacuumized, open the valve of gas cylinder or liquid charge pump, to being filled with environmental gas in pressure chamber or liquid reaches experimental pressure, open heating tape and muff (15) to environmental gas or heating liquid to experimental temperature;
Injecting step, with liquid charge pump or gas cylinder, inject drop or bubble by the adjustment precision needle-valve, by injection tubule (21), in environmental gas or liquid, form sizeable hanging drop or bubble, have retaining valve to prevent environmental gas or liquid backflow between injection tubule (21) and needle-valve;
Take pictures and calculation procedure, by CCD camera (41), observe shape, the size of drop or bubble, according to injection tubule (21) outside dimension, the scale parameter of taking pictures of CCD camera (41) is set, take the still photo of drop or bubble, calculate the physical size parameter of drop or bubble, the density difference that is aided with gas-liquid two-phase calculates interfacial tension.
5. the method that under a kind of high pressure claimed in claim 3, hanging drop or Bubbling method interfacial tension measurement mechanism carry out the interfacial tension measurement is characterized in that comprising the following steps:
Injection tubule position set-up procedure, unclamp and can regulate cutting ferrule, regulate the degree of depth of injection tubule (21) insertion pressure chamber's cylindrical shell (111), open backlight (42) and CCD camera (41), by CCD, observe the form center that the exit end face that makes to inject tubule is in the CCD camera, locking can be regulated cutting ferrule;
The experimental technique switch step, according to adopting hanging drop or Bubbling method, measure, supporting and the upper rotating metallic form pressure chamber (11) of locking device (31), while adopting sessile drop method, will inject tubule (21) rotation to top and surface level upright position, while adopting Bubbling method, will inject tubule (21) rotation to below and surface level upright position, and with clamping screw (313), that metal form pressure chamber (11) is fixing;
Form the hyperbaric environment step, close bleed valve (14), with vacuum pump, metal form pressure chamber (11) is vacuumized, open the valve of gas cylinder or liquid charge pump, to being filled with environmental gas in pressure chamber or liquid reaches experimental pressure, open heating tape and muff (15) to environmental gas or heating liquid to experimental temperature;
Injecting step, with liquid charge pump or gas cylinder, inject drop or bubble by the adjustment precision needle-valve, by injection tubule (21), in environmental gas or liquid, form sizeable hanging drop or bubble, have retaining valve to prevent environmental gas or liquid backflow between injection tubule and needle-valve;
Take pictures and calculation procedure, by CCD camera (41), observe shape, the size of drop or bubble, according to injection tubule (21) outside dimension, the scale parameter of taking pictures of CCD camera (41) is set, take the still photo of drop or bubble, calculate the physical size parameter of drop or bubble, the density difference that is aided with gas-liquid two-phase calculates interfacial tension.
CN2013103206872A 2013-07-26 2013-07-26 Interface tension measuring device and method by hanging drop or bubble blowing way under high pressure CN103411854A (en)

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CN104155217A (en) * 2014-07-17 2014-11-19 天津大学 High-temperature and high-pressure interfacial tension measurement device and method
CN104237077A (en) * 2014-09-22 2014-12-24 中国石油大学 Gas diffusion velocity measurement device and application thereof
CN104697900A (en) * 2013-12-05 2015-06-10 上海梭伦信息科技有限公司 Method for measuring interface tension and contact angle under vacuum controlled-temperature conditions, and apparatus thereof
CN105043936A (en) * 2015-07-08 2015-11-11 中国石油天然气股份有限公司 Device and method for measurement of contact angle and interfacial tension under simulative oil reservoir conditions
CN105092422A (en) * 2014-10-09 2015-11-25 天津科技大学 Portable temperature control surface tension meter
CN105203432A (en) * 2014-06-16 2015-12-30 上海梭伦信息科技有限公司 Device and method for testing contact angle and interfacial tension at ultrahigh pressure and high temperature
CN106018184A (en) * 2016-05-20 2016-10-12 大连理工大学 Experimental device for measuring dynamic contact angle under high-temperature and high-pressure environments
CN106053296A (en) * 2016-05-19 2016-10-26 江苏大学 Experiment platform for measuring solid-liquid interface contact angle under action of temperature gradient
CN107631961A (en) * 2016-07-18 2018-01-26 中国石油化工股份有限公司 Interface of oil and gas tension determining apparatus and method
CN107748221A (en) * 2017-08-23 2018-03-02 江苏大学 A kind of drop evaporation test device
CN107941616A (en) * 2017-12-10 2018-04-20 北京工业大学 A kind of sealing device that small size sample mechanical property is surveyed for Bubbling method
CN110286066A (en) * 2018-09-20 2019-09-27 中国科学院上海硅酸盐研究所 A kind of measuring device of sessile drop method measurement surface tension of high-temperature melt

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CN104697900A (en) * 2013-12-05 2015-06-10 上海梭伦信息科技有限公司 Method for measuring interface tension and contact angle under vacuum controlled-temperature conditions, and apparatus thereof
CN105203432A (en) * 2014-06-16 2015-12-30 上海梭伦信息科技有限公司 Device and method for testing contact angle and interfacial tension at ultrahigh pressure and high temperature
CN104155217A (en) * 2014-07-17 2014-11-19 天津大学 High-temperature and high-pressure interfacial tension measurement device and method
CN104237077B (en) * 2014-09-22 2016-08-24 中国石油大学(华东) A kind of gas diffusion velocity determinator and application
CN104237077A (en) * 2014-09-22 2014-12-24 中国石油大学 Gas diffusion velocity measurement device and application thereof
CN105092422A (en) * 2014-10-09 2015-11-25 天津科技大学 Portable temperature control surface tension meter
CN105043936A (en) * 2015-07-08 2015-11-11 中国石油天然气股份有限公司 Device and method for measurement of contact angle and interfacial tension under simulative oil reservoir conditions
CN105043936B (en) * 2015-07-08 2017-12-01 中国石油天然气股份有限公司 It is a kind of to simulate oil reservoir conditioned measurement contact angle and the device and method of interfacial tension
CN106053296B (en) * 2016-05-19 2018-11-09 江苏大学 A kind of experiment porch for solid-liquid face contact angle under measuring temperature gradient effect
CN106053296A (en) * 2016-05-19 2016-10-26 江苏大学 Experiment platform for measuring solid-liquid interface contact angle under action of temperature gradient
CN106018184B (en) * 2016-05-20 2018-08-21 大连理工大学 The experimental provision of dynamic contact angle is measured under a kind of high temperature and high pressure environment
CN106018184A (en) * 2016-05-20 2016-10-12 大连理工大学 Experimental device for measuring dynamic contact angle under high-temperature and high-pressure environments
CN107631961A (en) * 2016-07-18 2018-01-26 中国石油化工股份有限公司 Interface of oil and gas tension determining apparatus and method
CN107631961B (en) * 2016-07-18 2019-10-18 中国石油化工股份有限公司 Interface of oil and gas tension determining apparatus and method
CN107748221A (en) * 2017-08-23 2018-03-02 江苏大学 A kind of drop evaporation test device
CN107941616A (en) * 2017-12-10 2018-04-20 北京工业大学 A kind of sealing device that small size sample mechanical property is surveyed for Bubbling method
CN110286066A (en) * 2018-09-20 2019-09-27 中国科学院上海硅酸盐研究所 A kind of measuring device of sessile drop method measurement surface tension of high-temperature melt

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Application publication date: 20131127