CN109443251A - The test device and measurement method of high-temp solid material at high temperature contact angle - Google Patents
The test device and measurement method of high-temp solid material at high temperature contact angle Download PDFInfo
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- CN109443251A CN109443251A CN201811548440.5A CN201811548440A CN109443251A CN 109443251 A CN109443251 A CN 109443251A CN 201811548440 A CN201811548440 A CN 201811548440A CN 109443251 A CN109443251 A CN 109443251A
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- 238000012360 testing method Methods 0.000 title claims abstract description 46
- 239000011343 solid material Substances 0.000 title claims abstract description 23
- 238000000691 measurement method Methods 0.000 title claims abstract description 7
- 238000002844 melting Methods 0.000 claims abstract description 7
- 230000008018 melting Effects 0.000 claims abstract description 7
- 230000003287 optical effect Effects 0.000 claims abstract description 7
- 239000000523 sample Substances 0.000 claims description 72
- 229910052593 corundum Inorganic materials 0.000 claims description 29
- 239000010431 corundum Substances 0.000 claims description 29
- 229910006295 Si—Mo Inorganic materials 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000003780 insertion Methods 0.000 claims description 3
- 230000037431 insertion Effects 0.000 claims description 3
- 239000003870 refractory metal Substances 0.000 claims description 3
- 229910052594 sapphire Inorganic materials 0.000 claims description 3
- 239000010980 sapphire Substances 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 230000005619 thermoelectricity Effects 0.000 claims 2
- 230000007613 environmental effect Effects 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 10
- 238000001228 spectrum Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000012369 In process control Methods 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000010965 in-process control Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000010223 real-time analysis Methods 0.000 description 1
- 238000001304 sample melting Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/26—Measuring arrangements characterised by the use of optical techniques for measuring angles or tapers; for testing the alignment of axes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
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- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The test device and measurement method of consistent high-temp solid material at high temperature contact angle, device includes atmosphere control system, high temperature melting device, optical system and computer.The present invention has the characteristics that measuring accuracy is high, test scope is wide, high degree of automation and test repeatability are good to the measurement of high-temp solid material at high temperature contact angle.
Description
Technical field
The present invention relates to high-temp solid material, the especially a kind of test device and survey of high-temp solid material at high temperature contact angle
Amount method.
Background technique
In high-temp solid investigation of materials, contact angle is of great significance to material at high temperature performance study and application, but
Under hot environment, due to temperature gradient etc. in material physical chemistry variation and high temperature lower chamber, measurement observation material at high temperature
The test of superficial phenomenon is very difficult.And the high-performance that high-temperature atmosphere furnace is developed using international advanced technology is high energy-efficient new
Type electric furnace has the advantages of multiple atmospheres such as high vacuum, inert protective atmosphere, air atmosphere, oxygen atmosphere control, is that measurement is high
One of the important equipment of adiabator contact angle.
Chinese patent CN1265201C discloses the dress of a kind of on-line measurement surface tension of high-temperature melt, contact angle and density
It sets, using the data of sessile drop method measurement sample molten condition under the high temperature conditions, using improving instrument shooting precision and observation
The degree of automation realizes on-line testing result.Described in the patent specification, which cannot be to atmosphere in test process
It is controlled, therefore is not capable of measuring and needs vacuum/specific atmospheric conditions sample (such as part metals and high molecular material are in height
Under the conditions of warm air, chemical change occur causes test result inaccurate), the sample being only suitable only under test air conditions；Furthermore
The device of the invention leads to camera imaging to the disturbance of full spectrum light line due to high-temperature electric resistance furnace cavity inner temperature gradient during the test
There is error, it is difficult to measure the precise information of sample.
Therefore, the contact angle of high-temp solid material can be tested and realize that atmosphere is controllable, temperature control is smart by developing one kind
The high-temperature atmosphere furnace high, reproducible, automatization level is high is spent, the function of multi-use is realized, is current colleges and universities, scientific research institutions
Equal scientific research institutions' researching high-temperature solid material studies one of the equipment needed.
Summary of the invention
In order to overcome the above-mentioned prior art insufficient, the present invention provides a kind of test dress of high-temp solid material at high temperature contact angle
It sets and measurement method, the device has measuring accuracy height, test scope extensively, certainly to the measurement of high-temp solid material at high temperature contact angle
Dynamicization degree height and the good feature of test repeatability.
Technical solution of the invention is as follows:
A kind of test device of high-temp solid material at high temperature contact angle, it is characterized in that, which includes control climate system
System, high temperature melting device, optical system and computer, the atmosphere control system are storage cylinder, vacuum pump group and control climate
Cabinet, the high temperature melting device include air inlet, exhaust outlet, high-temperature corundum pipe furnace, Si-Mo rod, sample stage, thermocouple, described
Si-Mo rod be wound around the high-temperature corundum pipe furnace periphery, the both ends of the high-temperature corundum pipe furnace by seal assembly and
One end of refractory metal flange seal, the high-temperature corundum pipe furnace sets up air inlet and exhaust outlet separately up and down, and the center of the other end is set
Observation window is set, the sample stage is placed in the center flat-temperature zone of alundum furnace, and the lower surface center of the sample stage is upward
A circular groove is dug, the thermocouple is by the way that in the alundum tube furnace wall insertion circular groove, sample is placed in described
On sample stage；The sealing of the storage cylinder, control climate cabinet and air inlet is connected using stainless steel tube, it will with atmosphere triple valve
The vacuum pump is connected with gas outlet seal；The optical system includes high speed camera, background light source and light source controller,
The high speed camera is placed in outside the observation window of the alundum furnace, the sample, observation window and the high speed camera
It is co-located on the central axes of the alundum furnace；The background light source is below the high speed camera, the back
Scape light source is connected with the light source controller, the input terminal phase of the output end of the high speed camera and the computer
Even, the output end of the thermocouple is connected with the input terminal of the computer, an output end of the computer and
The control terminal of the electric control gear of the Si-Mo rod is connected, and the high speed camera is 6.5 times of high speed cameras continuously amplified, most
It is at high speed 2000 photos/second, data acquisition speed: 5G data/second；The observation window is made of sapphire material,
The control climate cabinet is made of pressure gauge, atmosphere three-way valve, gas flowmeter.
The storage cylinder includes air bottle, nitrogen cylinder, argon bottle, helium tank, the atmosphere of the high-temperature corundum pipe furnace
Control is selected by the control climate cabinet.
Using the test device of above-mentioned high-temp solid material at high temperature contact angle to the high temperature contact angle of high-temp solid material
Measurement method, including the following steps:
1) sample to be tested is placed on the sample stage, the high-temperature corundum pipe furnace is closed, according to be measured
Sample material situation, furnace chamber are interior by repeatedly vacuumizing-atmosphere cleaning, atmosphere test condition needed for reselection sample: air pressure
1.0 × 10-3-1.1×105Pa, inert atmosphere/vacuum/atmosphere, so that sample will not be because of testing environment during the test
It interferes and bring test error；
2) the high-temperature corundum pipe furnace described in is heated to hot conditions needed for sample to be tested, passes through the thermocouple survey close to sample
Amount temperature avoids the spacing due to thermocouple and sample to be tested by the heating of the computer control Si-Mo rod
From test error caused by the temperature difference of generation；
3) high speed camera described in simultaneously opens background light source, and the contour images data for acquiring sample high-resolution in real time simultaneously input
The computer；
4) data described in the computer stored described in, using the prior art carry out image procossing, obtain under high temperature to
The contact angle of sample.
High-temperature atmosphere furnace of the invention has the advantages that
1, test scope is wide.This test device using simple controllable control climate cabinet by pressure gauge, atmosphere three-way valve,
Gas flowmeter composition is wanted by adjusting pressure, gas flow and other selections, special atmosphere needed for can satisfy sample
(vacuum/air/argon/helium) is asked, chemically react sample will not under high temperature environment, object occurs so as to cause sample
Qualitative change or moieties variation, avoid the test error caused due to atmospheric factors.
2, test temperature is accurate.1700 DEG C of temperature upper limit, measuring accuracy reaches ± 1 DEG C, and central fovea is arranged below sample stage
Hole, temperature thermocouple, which is arranged in the central pit hole, to be put in inside sample stage, can both make sample stage furnace chamber just
The positioning of center flat-temperature zone, and closer to sample, avoid due to thermocouple and sample distance it is remote caused by test temperature error.
3, it is high precisely that data are obtained.Using the background light source by power-supply controller of electric brightness-adjustable, meet different sample tests
Demand avoids the measurement error that temperature gradient generates the disturbance of full spectrum light line in high temperature lower chamber.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the test device of high-temp solid material at high temperature contact angle of the present invention
Appended drawing reference: storage cylinder 1 (air, nitrogen, argon gas or helium are available), vacuum pump 2, control climate cabinet 3,
Air inlet 4, exhaust outlet 5, high-temperature corundum boiler tube 6, Si-Mo rod 7, sample stage 8, thermocouple 9, sample 10, high speed camera 11, background
Light source 12, light source controller 13, computer 14.
Specific embodiment
The present invention is further elaborated below with reference to embodiment and attached drawing:
First referring to Fig. 1, Fig. 1 is the structural schematic diagram of the test device of high-temp solid material at high temperature contact angle of the present invention,
As seen from the figure, the test device of high-temp solid material at high temperature contact angle of the present invention, including the makeup of atmosphere control system, high temperature melting
It sets, optical system and computer 14, the atmosphere control system is storage cylinder 1, vacuum pump group 2 and atmosphere control cabinet 3, described
High temperature melting device includes air inlet 4, exhaust outlet 5, high-temperature corundum pipe furnace 6, Si-Mo rod 7, sample stage 8, thermocouple 9, described
Si-Mo rod 7 is wound around 6 periphery of high-temperature corundum pipe furnace, passes through seal assembly at the both ends of the high-temperature corundum pipe furnace 6
With refractory metal flange seal, one end of the high-temperature corundum pipe furnace 6 sets up air inlet 4 and exhaust outlet 5 separately up and down, in the other end
Observation window (not shown) is arranged in the heart, and the sample stage 8 is placed in the center flat-temperature zone of high-temperature corundum pipe furnace 6, the sample
The lower surface center of sample platform 8 digs a circular groove upwards, and the thermocouple 9 passes through described in the insertion of 6 wall of high-temperature corundum pipe furnace
Circular groove in, sample 10 is placed on the sample stage 8；Using stainless steel tube by the storage cylinder 1, control climate cabinet
3 are connected with the sealing of air inlet 4, and the vacuum pump 2 is connected with the sealing of gas outlet 5 with atmosphere triple valve；The optical system
System includes high speed camera 11, background light source 12 and light source controller 13, and the high speed camera 11 is placed in the high-temperature corundum
Outside the observation window of pipe furnace 6, the sample 10, observation window and the high speed camera 11 are co-located in the high-temperature corundum pipe furnace
On 6 central axes；The background light source 12 is below the high speed camera 11, the background light source 12 and described
Light source controller 13 is connected, and the output end of the high speed camera 11 is connected with the input terminal of the computer 14, described
The output end of thermocouple 9 is connected with the input terminal of the computer 14, an output end of the computer 14 with it is described
Si-Mo rod 7 electric control gear control terminal be connected, the high speed camera 11 is 6.5 times of high speed cameras continuously amplified, most
It is at high speed 2000 photos/second, data acquisition speed: 5G data/second；The observation window is made of sapphire material,
The control climate cabinet is made of pressure gauge, atmosphere three-way valve, gas flowmeter.
The storage cylinder 1 includes air bottle, nitrogen cylinder, argon bottle, helium tank, the gas of the high-temperature corundum pipe furnace 6
Atmosphere selects control by the control climate cabinet 3.
Using the test device of above-mentioned high-temp solid material at high temperature contact angle to the high temperature contact angle of high-temp solid material
Measurement method, it is characterised in that: this method includes the following steps:
1) sample 10 is placed on the sample stage 8, the high-temperature corundum pipe furnace 6 is closed, according to be measured
Sample material situation, furnace chamber are interior by repeatedly vacuumizing-atmosphere cleaning, atmosphere test condition needed for reselection sample: air pressure
1.0 × 10-3-1.1×105Pa, inert atmosphere/vacuum/atmosphere, so that sample 10 will not be because of test wrapper during the test
It interferes and bring test error in border；
2) hot conditions needed for the high-temperature corundum pipe furnace 6 described in is heated to sample to be tested 10, pass through the heat close to sample 10
Galvanic couple 9 measures temperature, and the heating of the Si-Mo rod 7 is controlled by computer 14, avoid due to thermocouple with it is to be measured
Test error caused by the temperature difference that distance generates between sample；
3) high speed camera 11 described in simultaneously opens background light source 12, acquires the contour images data of 10 high-resolution of sample in real time
And input the computer 14；
4) computer 14 described in stores the data, carries out image procossing in the prior art, obtains under high temperature
The contact angle of sample 10.
Embodiment
Wavelength is used in this example as the ultra-blue-light of 470nm, avoids in high temperature lower chamber temperature gradient to full spectrum light
The measurement error that line disturbance generates；High speed camera 11 can be obtained with 6.5 times of continuous amplifications, 2000 photos of maximum speed/s, data
Take speed: 5G data/second；The storage of computer 14 or in real time analysis, provide a variety of automatic Matching Methods, and can automatically determine adherency
Function, baseline adjust the methods of automatic, manual, horizontal, curved surface.
Sample 10 is placed on sample stage 8 by the atmosphere control system, and sample 10, observation window (are not marked in figure
Out) and high speed camera 11 is in same level, to obtain high image quality degradation；Observation window, thermocouple 9 and high-temperature corundum pipe furnace
Using the metal flange sealing fastening for meeting DN 40ISO KF standard at 6, so that high-temperature electric resistance furnace cavity is in a seal shape
State；Using vacuum pump 2 (mechanical pump and molecular pump or diffusion pump, secondary vacuum system do not mark in figure) at room temperature from exhaust
5 pumping high vacuums of mouth make high-temperature electric resistance furnace cavity reach a sample by storage cylinder 1 further according to material particularity in 4 air inlet of air inlet
Atmospheric condition needed for product 10.
In process control temperature-rise period, temperature change is measured using the thermocouple 9 for being close to sample 10；Computer and high speed
Camera is connected, and can observe sample melted dynamic process in real time；It selects industrial cold light source as background light source, avoids under high temperature
The measurement error that cavity inner temperature gradient generates the disturbance of full spectrum light line；After sample melting, high speed camera 11 can be obtained clearly
Image, the variation that entire sample profile image occurs can be with captured in real-time (2000 photos of maximum speed/s), and are stored in meter
In calculation machine 14；Image procossing calculating is carried out according to resulting clear contour images starting software, a variety of automatic Fittings are provided
Method, and can automatically adjust, obtain the contact angle and fusing sample of the solids such as metal under high temperature, alloy, ceramics, clinker.
Experiment shows that the present invention has measuring accuracy height, test scope to the measurement of high-temp solid material at high temperature contact angle
Extensively, high degree of automation and the good feature of test repeatability.
The contents of the present invention are not limited to cited by embodiment, and those of ordinary skill in the art are by reading description of the invention
And to any equivalent transformation that technical solution of the present invention is taken, all are covered by the claims of the invention.
Claims (3)
1. a kind of test device of high-temp solid material at high temperature contact angle, which is characterized in that the device include atmosphere control system,
High temperature melting device, optical system and computer (14), the atmosphere control system is storage cylinder (1), vacuum pump group (2) is gentle
Atmosphere control cabinet (3), the high temperature melting device include air inlet (4), exhaust outlet (5), high-temperature corundum pipe furnace (6), Si-Mo rod
(7), sample stage (8), thermocouple (9), the Si-Mo rod (7) is wound around high-temperature corundum pipe furnace (6) periphery, described
High-temperature corundum pipe furnace (6) both ends by seal assembly and refractory metal flange seal, the one of the high-temperature corundum pipe furnace (6)
End sets up air inlet (4) and exhaust outlet (5) separately up and down, and observation window is arranged in the center of the other end, and the sample stage (8) is placed in corundum
The center flat-temperature zone of pipe furnace (6), the lower surface center of the sample stage (8) dig a circular groove, the heat upwards
Galvanic couple (9) is by the way that in high-temperature corundum pipe furnace (6) the wall insertion circular groove, sample (10) is placed in the sample stage (8)
On；The storage cylinder (1), control climate cabinet (3) are connected with air inlet (4) sealing using stainless steel tube, with atmosphere threeway
The vacuum pump (2) is connected by valve with gas outlet (5) sealing；The optical system includes high speed camera (11), bias light
Source (12) and light source controller (13), the high speed camera (11) is placed in outside the observation window of the alundum furnace (6), described
Sample (10), observation window and the high speed camera (11) be co-located on the central axes of the alundum furnace (6)；Described
Background light source (12) is below the high speed camera (11), the background light source (12) and the light source controller
(13) it is connected, the output end of the high speed camera (11) is connected with the input terminal of the computer (14), the thermoelectricity
The output end of even (9) is connected with the input terminal of the computer (14), an output end of the computer (14) and institute
The control terminal of the electric control gear for the Si-Mo rod (7) stated is connected, and the high speed camera (11) is 6.5 times of high speed phases continuously amplified
Machine, maximum speed are 2000 photos/second, data acquisition speed: 5G data/second；The observation window uses sapphire material
It is made, the control climate cabinet (3) is made of pressure gauge, atmosphere three-way valve, gas flowmeter.
2. the test device of high-temp solid material at high temperature contact angle according to claim 1, it is characterised in that the storage
Gas cylinder (1) includes air bottle, nitrogen cylinder, argon bottle, helium tank, and the atmosphere of the high-temperature corundum pipe furnace (6) is by the gas
Atmosphere control cabinet (3) selection control.
3. utilizing the test device of high-temp solid material at high temperature contact angle described in claim 1 to the high temperature of high-temp solid material
The measurement method of contact angle, it is characterised in that: this method includes the following steps:
1) sample (10) is placed on the sample stage (8), closes the high-temperature corundum pipe furnace (6), according to
Sample material situation, furnace chamber are interior by repeatedly vacuumizing-atmosphere cleaning, atmosphere test condition needed for reselection sample: gas
It is pressed in 1.0 × 10-3-1.1×105Pa, inert atmosphere/vacuum/atmosphere, so that sample (10) will not be because of surveying during the test
Try environmental disturbances and bring test error；
2) hot conditions needed for the high-temperature corundum pipe furnace (6) described in is heated to sample to be tested (10), by close to sample (10)
Thermocouple (9) measures temperature, by the heating of computer (14) control Si-Mo rod (7), avoids due to thermoelectricity
Test error caused by the temperature difference that distance generates between idol and sample to be tested；
3) high speed camera (11) described in simultaneously opens background light source 12, acquires the contour images data of sample (10) high-resolution in real time
And input the computer (14)；
4) data described in computer (14) storage described in, starting software carry out image procossing, obtain sample under high temperature
(10) contact angle.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110274850A (en) * | 2019-07-30 | 2019-09-24 | 西南交通大学 | A kind of contact angle test device and test method |
| CN112162079A (en) * | 2020-09-09 | 2021-01-01 | 中国科学院过程工程研究所 | Unattended testing system device and testing method for thermophysical parameters of melt |
| CN114459959A (en) * | 2021-12-30 | 2022-05-10 | 北京工业大学 | Device and method for measuring high-temperature contact angle of material surface |
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| CN114459959B (en) * | 2021-12-30 | 2023-12-08 | 北京工业大学 | Device and method for measuring high-temperature contact angle of material surface |
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