CN104089972B - Method for determining condensate depression of metal micro-drops during rapid solidification process and device used by method - Google Patents
Method for determining condensate depression of metal micro-drops during rapid solidification process and device used by method Download PDFInfo
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Abstract
The invention provides a method for determining condensate depression of metal micro-drops during a rapid solidification process and a device used by the method, belonging to the technical field of metal physical performance test. The method comprises the following steps: firstly, preparing metal microparticle liquid drops by using a pulse micro-pore method; then respectively determining temperatures of the metal microparticle liquid drops dropping into oil at a starting moment and a balancing moment from different positions in a falling process; and finally, carrying out heat balance calculation to obtain liquid phase content, nucleation temperature and condensate depression of the metal microparticle liquid drops at different positions. The device used by the method comprises a vacuum system, a liquid drop spraying system, an image acquisition system and a liquid drop temperature testing system, wherein the liquid drop temperature testing system is mounted in a vacuum system; the liquid drop spraying system is mounted above the liquid drop temperature testing system; the image acquisition system is connected to a vacuum cavity of the vacuum system. The method can be used for monitoring and determining the condensate depression of the metal micro-drops during the rapid solidification process in real time; the device solves the problem of existing thermal analytical equipment that the rapid solidification process cannot be tested in real time due to low cooling speed.
Description
Technical field
The invention belongs to Physical Property of Metal technical field of measurement and test, particularly to a kind of survey of rapid solidification metal degree of supercooling
Determine method, additionally relate to it and measure device.
Background technology
No container rapid solidification is under faster rate of cooling during than common process, makes metal and alloy with pole
Fast speed is changed into the process of solid-state from liquid, and this process much deviates equilibrium state, to the forming core in process of setting and solidification
Tissue morphology afterwards has significant effect it is expected to obtain the tissue that composition is uniform, crystal grain is tiny.
Micropartical prepared by pulse MP method (POEM) has the features such as in the same size, sphericity is high, and because drop fall
The process that falls is no container rapid solidification, it is to avoid drop leads to the generation of the uncontrollable factors such as heterogeneous forming core because of wall induction, from
And it is further ensured that the Warm status of droplet solidification process unanimously, finally give the consistent uniform-spherical micropartical of microstructure.
Degree of supercooling is the important characterization parameter of rapid solidification, by the reasonable solidification degree of supercooling controlling melt, permissible
Obtain the solidified structure of different shape, and obtain different material properties.Therefore, how the degree of supercooling of rapid solidification is entered
It is key therein that row is evaluated with sign.
However, usual metal degree of supercooling can be carried out using the means such as differential scanning calorimetry (DSC) or thermal analyzer (DTA)
Measurement, but can only be just to carry out after material preparation completes, and due to equipment limitation, metal bath rate of cooling is all not
Height is it is impossible to test to the degree of supercooling of rapid solidification.
Content of the invention
It is an object of the invention to provide a kind of method measuring metal droplet rapid solidification degree of supercooling and its device, use first
Pulse MP method prepares molten drop, and then the diverse location in drop whereabouts track fixes thermos flask calorie meter, flat by heat
Weighing apparatus analysis obtains the liquid content in various location for the microdroplet, and then obtains drop forming core point, then obtains shape by Theoretical Calculation
Nuclear temperature and degree of supercooling, accordingly assay method devise the corollary equipment of mensure, the method for the present invention can be with real-time monitoring metal
The degree of supercooling of microdroplet rapid solidification, this invention device solves that existing thermal analyzer rate of cooling is not high cannot be to rapid solidification
Process carries out the limitation of real-time testing.
The present invention be employed technical scheme comprise that for achieving the above object：A kind of mensure metal droplet rapid solidification degree of supercooling
Method it is characterised in that：Prepare metal microparticle drop initially with pulse MP method；Then under metal microparticle drop
The metal microparticle drop start time falling in oil and the temperature balancing the moment are measured respectively on the diverse location during falling；
The liquid content of various location metal microparticle drop is subsequently obtained by heat Balance Calculation；Liquid content is finally recycled to lead to
Cross nucleation temperature and the degree of supercooling that Theoretical Calculation obtains metal microparticle drop.
Methods described includes sequential steps in detail below：
(1) pulse MP method prepares metal microparticle drop
Foraminate potsherd will be carried to be fixed on crucible bottom, to crucible and vacuum cavity evacuation, and be filled with inertia guarantor
Shield gas, becomes molten condition using heater heating crucible to its interior metal；It is passed through noble gases in crucible, make vacuum chamber
Body and crucible reach stable differential pressure；Certain pulse signal is applied to piezoelectric ceramics so as to drive driving rod to produce one longitudinally
Micro-displacement, this displacement acts on the metal bath of crucible bottom, so that metal bath is sprayed from crucible bottom aperture and forms metal
Micropartical drop, piezoelectric ceramics often moves once, can form a metal microparticle drop at aperture；
(2) measure the temperature falling in oil
After metal microparticle droplets stable, thermos flask calorie meter is fixed on a certain height of metal microparticle drop whereabouts
Degree, removes the diaphragm seal on microdroplet ingate, moves into immediately after metal microparticle drop falls in the oil of thermos flask calorie meter
Diaphragm seal, stops metal injection micropartical drop simultaneously, when record metal microparticle drop falls into starting in oil and falls into respectively
Carve and balance the temperature of oil in moment thermos flask calorie meter；
(3) calculate liquid content
Repeat step (2) obtain various location metal microparticle drop fall into starting in oil fall into the moment and balance when
Carve the temperature of oil in thermos flask calorie meter, obtain the liquid content in various location for the microdroplet through heat Balance Calculation；
(4) calculate degree of supercooling
Using the liquid content of various location, obtain nucleation temperature and the mistake of metal microparticle drop by Theoretical Calculation
Cold degree.
Described step (1) pulse MP method is prepared specific technological process and parameter in metal microparticle drop and is included：
1) feed：Foraminate potsherd will be carried to be fixed on crucible bottom, open lid on crucible, adding in crucible needs
The metal material of measurement, and seal；
2) evacuation：It is evacuated to vacuum using mechanical pump and diffusion pump to crucible and vacuum cavity to be not higher than
0.001Pa, and it is filled with inert protective gas Ar, it is repeated, finally make pressure in vacuum cavity reach an atmospheric pressure；
3) fusing metal：Heating crucible, using the metal material in heater fusion crucible, and uses thermocouple real-time monitoring
Temperature in crucible, metal material is incubated 10-30 minute after being completely melt；
4) impulse jet：Noble gases are passed through in crucible by crucible air inlet pipe, make to reach between crucible and vacuum cavity
To stablizing differential pressure 0-50kPa, using signal generator edit pulse signal and be applied to piezoelectric ceramics, piezoelectric ceramics is believed in pulse
Number driving under produce micro-displacement, and drive transmission rod motion, this micro-displacement acts on the gold of crucible bottom by driving rod
Belong to melt, so that metal microparticle drop projects from aperture；
5) obtain symmetrical liquid drop：Computer utilizes computer image analysis software, and the metal according to captured by ccd video camera is micro-
Particle drop image calculates the diameter of metal microparticle drop, frequency that feedback adjustment agitator produces, waveform parameter, thus
Obtain the homogeneous metal micropartical drop being sized.
A kind of device of being adopted of method measuring metal droplet rapid solidification degree of supercooling it is characterised in that：This device bag
Include vacuum system, liquid droplet ejection system, image capturing system and drop Research on Automatic Measuring System of Temperature, described drop Research on Automatic Measuring System of Temperature peace
It is loaded on inside vacuum system, liquid droplet ejection system is installed on the surface of drop Research on Automatic Measuring System of Temperature, image capturing system connects
On the vacuum cavity of vacuum system.
Described vacuum system includes vacuum cavity, mechanical pump and diffusion pump, and diffusion pump is installed on vacuum chamber body sidewall,
Mechanical pump is connected on diffusion pump, and vacuum cavity is also equipped with cavity air inlet pipe and crucible air inlet pipe.
Described liquid droplet ejection system is fixedly installed in inside vacuum cavity using crucible, and center has the pottery of circular aperture
Piece is fixedly installed in crucible bottom, driving rod lower end be located at potsherd upper surface, driving rod upper end sequentially pass through crucible top and
Vacuum cavity top is connected with piezoelectric ceramics, and piezoelectric ceramics is connected with signal generator, and signal generator is connected with computer；Institute
State crucible periphery install having heaters, temperature-control heat couple be located at crucible inside, temperature controller respectively with temperature-control heat couple, heating
Device connects, and the temperature controller other end is connected with computer.
, between 0.020-1.500mm, the frequency of vibration of described piezoelectric ceramics is in 1Hz-2kHz for described small aperture scope
Between.
Described drop Research on Automatic Measuring System of Temperature is movably installed on vacuum chamber body sidewall using bracing frame, and outer heat screen is fixed on
On bracing frame, interior heat screen is fixed on inside outer heat screen, forms thermal-insulating chamber, interior thermal insulation between outer heat screen and interior heat screen
Screen upper opening, and it is internally formed soak chamber, adiabatic closure is installed on interior heat screen upper opening, adiabatic sealing
Lid center has microdroplet ingate, and microdroplet ingate is located at immediately below aperture, is stamped diaphragm seal, diaphragm seal above microdroplet ingate
It is movably installed on vacuum cavity by support, temperature thermocouple is located inside soak chamber, temperature measurer is connected to thermometric heat
The galvanic couple other end, temperature measurer is connected with computer.
Described image acquisition system is installed on vacuum chamber body sidewall using ccd video camera, and image pick-up card is taken the photograph with CCD
Camera is connected, and computer is connected with image pick-up card.
There is plate washer, described plate washer is movably installed in upper bracket between described liquid droplet ejection system and drop Research on Automatic Measuring System of Temperature
On, upper bracket is movably installed on vacuum chamber body sidewall.
The method of the present invention and its device have following beneficial effect：
(1) method and device of actual measured amount metal droplet rapid solidification degree of supercooling when provided by the present invention a kind of, by arteries and veins
Rush micropore spraying technique to combine with thermos flask Calorimetry system, when actual measured amount drop rapid solidification forming core point, overcome
Existing thermal analyzer rate of cooling not high it is impossible to the degree of supercooling of rapid solidification is carried out with the limitation of real-time testing.
(2) device that the present invention provides is sprayed by pulse small hole and produces the homogeneous controlled molten drop of size, and technique can
Control property is strong, and the hot resume of drop are consistent, adjusts the parameter of signal generator especially with image capturing system, reduces molten drop
Error with setting drop size, improves the degree of accuracy of calculating.
(3) the drop descent that the inventive method passes through the injection generation of pulse micropore is no container rapid solidification, it is to avoid
Drop leads to the generation of the uncontrollable factors such as heterogeneous forming core because of wall induction, thus be further ensured that the heat of droplet solidification process
State consistency, finally gives the consistent uniform-spherical micropartical of microstructure, and continuous mode is repeatable strong.
Brief description
Fig. 1 is the apparatus structure schematic diagram that a kind of method measuring metal droplet rapid solidification degree of supercooling adopts.
In figure：1 piezoelectric ceramics, 2 driving rods, 3 crucibles, 4 heaters, 5 temperature-control heat couple, 6 metal baths, 7 vacuum cavities,
8 apertures, 9 potsherds, 10 metal microparticle drops, 11 plate washers, 12 upper brackets, 13 signal generators, 14 temperature controllers, 15 electricity
Brain, 16 image pick-up cards, 17CCD video camera, 18 temperature measurers, 19 temperature thermocouples, 20 diaphragm seals, 21 microdroplet ingates, 22 is exhausted
Heat seal lid, 23 outer heat screens, 24 thermal-insulating chambers, heat screen in 25,26 oil, 27 bracing frames, 28 supports, 29 diffusion pumps, 30 machineries
Pump, 31 cavity air inlet pipe, 32 crucible air inlet pipe.
Specific embodiment
Below in conjunction with accompanying drawing, the present invention will be further described, but the invention is not limited in specific embodiment.
Embodiment 1
The device that a kind of method of mensure metal droplet rapid solidification degree of supercooling as shown in Figure 1 is adopted, this device bag
Include vacuum system, liquid droplet ejection system, image capturing system and drop Research on Automatic Measuring System of Temperature, described drop Research on Automatic Measuring System of Temperature peace
It is loaded on inside vacuum system, liquid droplet ejection system is installed on the surface of drop Research on Automatic Measuring System of Temperature, image capturing system connects
On the vacuum cavity of vacuum system.
Vacuum system includes vacuum cavity 7, mechanical pump 30 and diffusion pump 29, diffusion pump be installed on vacuum chamber body sidewall it
On, mechanical pump is connected on diffusion pump, and vacuum cavity is also equipped with cavity air inlet pipe 31 and crucible air inlet pipe 32, evacuation
Before, by valve closing cavity air inlet pipe and crucible air inlet pipe, the vacuum in vacuum cavity can reach below 10-3Pa.
Liquid droplet ejection system is fixedly installed in inside vacuum cavity 7 using crucible 3, and center has the pottery of circular aperture 8
Piece 9 is fixedly installed in crucible bottom, and driving rod 2 lower end is located at potsherd upper surface, and driving rod upper end sequentially passes through crucible top
It is connected with piezoelectric ceramics 1 with vacuum cavity top, small aperture is 0.020mm, the frequency of vibration of piezoelectric ceramics, in 2000Hz, is pressed
Electroceramics is connected with signal generator 13, and signal generator is connected with computer 15；Described crucible periphery installs having heaters 4,
Temperature-control heat couple 5 is located inside crucible, and temperature controller 14 is connected with temperature-control heat couple, heater respectively, and temperature controller is another
One end is connected with computer.
Drop Research on Automatic Measuring System of Temperature is movably installed on vacuum chamber body sidewall using bracing frame, and outer heat screen is fixed on support
On frame, interior heat screen is fixed on inside outer heat screen, forms thermal-insulating chamber, in interior heat screen between outer heat screen and interior heat screen
Portion's opening, and it is internally formed soak chamber, adiabatic closure is installed on interior heat screen upper opening, in adiabatic closure
The heart has microdroplet ingate, and microdroplet ingate is located at immediately below aperture, is stamped diaphragm seal, diaphragm seal passes through above microdroplet ingate
Support is movably installed on vacuum cavity, and temperature thermocouple is located inside soak chamber, and temperature measurer is connected to temperature thermocouple
The other end, temperature measurer is connected with computer.
Image capturing system is installed on vacuum chamber body sidewall using ccd video camera, image pick-up card and ccd video camera
It is connected, computer is connected with image pick-up card.
There is plate washer 11, described plate washer is movably installed in upper bracket 12 between liquid droplet ejection system and drop Research on Automatic Measuring System of Temperature
On, upper bracket 12 is movably installed on vacuum chamber body sidewall.
Measure the degree of supercooling of metal droplet rapid solidification using said method, including sequential steps in detail below：
1st, pulse MP method prepares metal microparticle drop
(1) feed：Potsherd 9 with aperture 8 is fixed on crucible 3 bottom, opens lid on crucible 3, add in crucible 3
Enter to need the metal material of measurement, and seal；
(2) evacuation：Being evacuated to vacuum using mechanical pump 30 and diffusion pump 29 to crucible 3 and vacuum cavity 7 is
0.001Pa, and it is filled with inert protective gas Ar, it is repeated, finally make pressure in vacuum cavity 7 reach an atmospheric pressure；
(3) fusing metal：Heating crucible 3, using the metal material in heater 4 fusion crucible 3, and uses temperature-control heat couple
Temperature in 5 real-time monitoring crucibles 3, metal material is incubated 10 minutes after being completely melt；
(4) impulse jet：Noble gases are passed through in crucible 3 by crucible air inlet pipe 32, make crucible 3 and vacuum cavity 7
Between reach stable differential pressure 50kPa, using signal generator 13 edit pulse signal and be applied to piezoelectric ceramics 1, piezoelectric ceramics 1
Produce micro-displacement under the driving of pulse signal, and drive driving rod 2 to move, this micro-displacement acts on earthenware by driving rod 2
The metal bath 6 of crucible 3 bottom, so that metal microparticle drop 10 projects from aperture 8；
(5) obtain symmetrical liquid drop：Computer 15 utilizes computer image analysis software, according to captured by ccd video camera 17
Metal microparticle drop image calculates the diameter of metal microparticle drop, and the frequency that feedback adjustment agitator produces, waveform are joined
Number, thus obtain the homogeneous metal micropartical drop being sized.
2nd, measure the temperature falling in oil
After metal microparticle droplets stable, by thermos flask calorie meter be fixed in metal microparticle drop descent path away from
The distance of crucible 3 small hole at bottom part 8 is on the height and position of H, removes the diaphragm seal 20 on microdroplet ingate 21, removes plate washer simultaneously
11, move into diaphragm seal 20 immediately after n metal microparticle drop falls in the oil of thermos flask calorie meter, stop injection gold simultaneously
Belong to micropartical drop, computer respectively real time record metal microparticle drop fall into starting in oil fall into the moment temperature be TiWith
In balance moment thermos flask calorie meter, the temperature of oil is Tf；
3rd, calculate liquid content
Repeat step (2) obtain various location metal microparticle drop fall into starting in oil fall into the moment and balance when
Carve the temperature of oil in thermos flask calorie meter.
Measuring metal microparticle drop whereabouts initial velocity by ccd video camera 17 is v.
The resistance that metal microparticle drop (hereinafter referred to as drop) whereabouts is subject to is directly proportional to speed, and k is resistance coefficient.
F=k v (1)
According to Newton's second law
Integrate：
Wherein, m is drop mass, and d is liquid-drop diameter, and ρ is drop density, and v is liquid drop speed, H drop away from aperture 8 away from
From.
Do not consider forming core and latent heat, drop temperature is over time：
T=T∞-(T∞-T0)e-mt(6)
Wherein：T∞For ambient temperature, T0For drop initial temperature, Re is Reynolds number, and Pr is Prandtl constant, and λ g is gas
Thermal conductivity, ρgFor the density of gas, μgViscosity for gas.
It is calculated convection transfer rate h using (8)-(10) formula, then is brought in (6) and (7), you can obtain ignoring shape
The drop cooling curve T～t of core and latent heat.
Thermos flask calorie meter is fixed at distance of fall H, and the oily initial temperature obtaining, equilibrium temperature are respectively Ti、Tf, use
Formula (11) calculates and comprises liquid content x in corresponding drop.
X=[m0C0(Tf-Ti)-mtCd(Te-Tf)]/mtΔHf(11)
Wherein：m0It is the quality of oil；C0It is oily specific heat capacity；mtIt is drop gross mass；CdIt is drop specific heat capacity；TeIt is that drop is common
Brilliant temperature, Δ HfIt is balanced melt latent heat；
Fall into temperature T that starting in oil falls into the moment using the drop obtaining at differing heightsiWith the insulation of balance moment
Temperature T of oil in bottle calorie meterf, liquid content x at different distance of fall H for the drop can be obtained, fitted to by experimental point
Curve, as shown below：
Relation between drop distance of fall and liquid content
4th, calculate degree of supercooling
Using the pass between the liquid content of various location in step 3 and the drop distance of fall of matching and liquid content
It is curve, the flex point obtaining in figure is forming core point, corresponding H0For nucleation site.By H0Substitute into the formula (5) in step 3, obtain
Drop forming core point corresponding time t0, then by t0Bring in formula (6), obtain nucleation temperature Tn, then degree of supercooling Δ T=Te-Tn.
Embodiment 2
Embodiment 2 is identical with device in embodiment 1 and assay method, and the different relevant parameter of this apparatus and method is such as
Under：
(1) in this device, the aperture of aperture 8 is 0.150mm, and the frequency of vibration of piezoelectric ceramics is 700Hz；
(2) step 1, pulse MP method prepare (2) evacuation in metal microparticle drop：Using mechanical pump 30 and diffusion pump
29 pairs of crucibles 3 and vacuum cavity 7 are evacuated to vacuum for 0.0009Pa；
(3) step 1, pulse MP method prepare (3) fusing metal in metal microparticle drop：After metal material is completely melt
Insulation 20 minutes；
(4) step 1, pulse MP method prepare (4) impulse jet in metal microparticle drop：By crucible air inlet pipe 32 to
It is passed through noble gases in crucible 3, make to reach stable differential pressure 20kPa between crucible 3 and vacuum cavity 7.
Embodiment 3
Embodiment 3 is identical with device in embodiment 1 and assay method, and the different relevant parameter of this apparatus and method is such as
Under：
(1) in this device, small aperture is 1.500mm, and the frequency of vibration of piezoelectric ceramics is 1Hz；
(2) step 1, pulse MP method prepare (2) evacuation in metal microparticle drop：Using mechanical pump 30 and diffusion pump
29 pairs of crucibles 3 and vacuum cavity 7 are evacuated to vacuum for 0.0007Pa；
(3) step 1, pulse MP method prepare (3) fusing metal in metal microparticle drop：After metal material is completely melt
Insulation 30 minutes；
(4) step 1, pulse MP method prepare (4) impulse jet in metal microparticle drop：By crucible air inlet pipe 32 to
It is passed through noble gases in crucible 3, make to reach stable differential pressure 0kPa between crucible 3 and vacuum cavity 7.
Claims (8)
1. a kind of measure metal droplet rapid solidification degree of supercooling method it is characterised in that：Initially with the preparation of pulse MP method
Metal microparticle drop；Then measure metal microparticle liquid respectively on the diverse location in metal microparticle drop dropping process
It is dropped into the start time in oil and the temperature balancing the moment；Subsequently various location metal particle is obtained by heat Balance Calculation
The liquid content of sub- drop；Finally recycle liquid content pass through Theoretical Calculation obtain the nucleation temperature of metal microparticle drop with
Degree of supercooling；
Including sequential steps in detail below：
1) pulse MP method prepares metal microparticle drop
Potsherd (9) with aperture (8) is fixed on crucible (3) bottom, to crucible (3) and vacuum cavity (7) evacuation, and
It is filled with inert protective gas, become molten condition using heater (4) heating crucible (3) to its interior metal；Logical in crucible (3)
Enter noble gases, make vacuum cavity (7) and crucible (3) reach stable differential pressure；Piezoelectric ceramics (1) is applied with certain pulse letter
Number so as to drive driving rod (2) to produce a longitudinal micro-displacement, this displacement acts on the metal bath (6) of crucible (3) bottom,
So that metal bath is sprayed from crucible (3) small hole at bottom part (8) and form metal microparticle drop (10), piezoelectric ceramics (1) often moves one
Secondary, a metal microparticle drop (10) can be formed at aperture；
2) measure the temperature falling in oil
After metal microparticle droplets stable, thermos flask calorie meter is fixed on a certain height of metal microparticle drop whereabouts,
Remove the diaphragm seal (20) on microdroplet ingate (21), after metal microparticle drop falls in the oil of thermos flask calorie meter immediately
Move into diaphragm seal (20), stop metal injection micropartical drop simultaneously, record metal microparticle drop falls into opening in oil respectively
Begin to fall into the temperature of oil in moment and balance moment thermos flask calorie meter；
3) calculate liquid content
Repeat step 2) obtain various location metal microparticle drop fall into starting in oil fall into the moment and balance the moment protect
In warm bottle calorie meter, the temperature of oil, obtains the liquid content in various location for the microdroplet through heat Balance Calculation；
4) calculate degree of supercooling
Using the liquid content of various location, the nucleation temperature of metal microparticle drop and supercool is obtained by Theoretical Calculation
Degree.
2. according to claim 1 a kind of measure metal droplet rapid solidification degree of supercooling method it is characterised in that：Described
Step 1) in specific technological process and parameter include：
1) -1 charging：Potsherd (9) with aperture (8) is fixed on crucible (3) bottom, opens the upper lid of crucible (3), in crucible
(3) adding in needs the metal material of measurement, and seals；
1) -2 evacuation：Using mechanical pump (30) and diffusion pump (29), vacuum is evacuated to crucible (3) and vacuum cavity (7)
Not higher than 0.001Pa, and it is filled with inert protective gas Ar, it is repeated, finally make the interior pressure of vacuum cavity (7) reach one greatly
Air pressure；
1) -3 fusing metal：Heating crucible (3), using the metal material in heater (4) fusion crucible (3) and hot with temperature control
Temperature in galvanic couple (5) real-time monitoring crucible (3), metal material is incubated 10-30 minute after being completely melt；
1) -4 impulse jet：Noble gases are passed through in crucible (3) by crucible air inlet pipe (32), make crucible (3) and vacuum chamber
Body reaches stable differential pressure 0-50kPa between (7), using signal generator (13) edit pulse signal and be applied to piezoelectric ceramics
(1), piezoelectric ceramics (1) produces micro-displacement under the driving of pulse signal, and drives driving rod (2) to move, this micro-displacement
Act on the metal bath (6) of crucible (3) bottom by driving rod (2), so that metal microparticle drop (10) is from aperture (8)
Middle injection；
1) -5 acquisition symmetrical liquid drop：Computer (15) utilizes computer image analysis software, according to captured by ccd video camera (17)
Metal microparticle drop image calculates the diameter of metal microparticle drop, and the frequency that feedback adjustment agitator produces, waveform are joined
Number, thus obtain the homogeneous metal micropartical drop being sized.
3. the device that a kind of method measuring metal droplet rapid solidification degree of supercooling according to claim 1 is adopted, its
It is characterised by：This device includes vacuum system, liquid droplet ejection system, image capturing system and drop Research on Automatic Measuring System of Temperature, described
Drop Research on Automatic Measuring System of Temperature is installed on inside vacuum system, and liquid droplet ejection system is installed on just going up of drop Research on Automatic Measuring System of Temperature
Side, image capturing system is connected on the vacuum cavity of vacuum system；
Described drop Research on Automatic Measuring System of Temperature is movably installed on the wall of vacuum cavity (7) side using bracing frame (27), outer heat screen
(23) be fixed on bracing frame (27), interior heat screen (25) is fixed on inside outer heat screen, outer heat screen and interior heat screen it
Between form thermal-insulating chamber (24), interior heat screen upper opening, and it is internally formed soak chamber, in adiabatic closure (22) is installed on
On heat screen upper opening, adiabatic closure center has microdroplet ingate (21), microdroplet ingate be located at aperture (8) just under
Side, is stamped diaphragm seal (20), diaphragm seal is movably installed on vacuum cavity by support (28), thermometric above microdroplet ingate
Thermocouple (19) is located inside soak chamber, and temperature measurer is connected to the temperature thermocouple other end, and temperature measurer is connected with computer.
4. the device that a kind of method measuring metal droplet rapid solidification degree of supercooling according to claim 3 is adopted, its
It is characterised by：Described vacuum system includes vacuum cavity (7), mechanical pump (30) and diffusion pump (29), and diffusion pump is installed on vacuum
On the wall of cavity (7) side, mechanical pump is connected on diffusion pump, and vacuum cavity is also equipped with cavity air inlet pipe (31) and crucible
Air inlet pipe (32).
5. the device that a kind of method measuring metal droplet rapid solidification degree of supercooling according to claim 3 is adopted, its
It is characterised by：Described liquid droplet ejection system is fixedly installed in vacuum cavity (7) inside using crucible (3), and center has circular little
The potsherd (9) in hole (8) is fixedly installed in crucible (3) bottom, and driving rod (2) lower end is located at potsherd upper surface, on driving rod
End is sequentially passed through crucible top and is connected with piezoelectric ceramics (1) with vacuum cavity top, piezoelectric ceramics and signal generator (13) phase
Connect, signal generator is connected with computer；Described crucible periphery installs having heaters (4), and temperature-control heat couple (5) is located in crucible
Portion, temperature controller (14) is connected with temperature-control heat couple, heater respectively, and temperature controller (14) other end is with computer (15) even
Connect.
6. the device that a kind of method measuring metal droplet rapid solidification degree of supercooling according to claim 5 is adopted, its
It is characterised by：Between 0.020-1.500mm, the frequency of vibration of described piezoelectric ceramics (1) exists described aperture (8) pore diameter range
Between 1Hz-2kHz.
7. the device that a kind of method measuring metal droplet rapid solidification degree of supercooling according to claim 3 is adopted, its
It is characterised by：Described image acquisition system is installed on the wall of vacuum cavity (7) side using ccd video camera (17), image acquisition
Card (16) is connected with ccd video camera (17), and computer (15) is connected with image pick-up card.
8. the device that a kind of method measuring metal droplet rapid solidification degree of supercooling according to claim 3 is adopted, its
It is characterised by：There is plate washer (11), described plate washer is movably installed between described liquid droplet ejection system and drop Research on Automatic Measuring System of Temperature
On upper bracket (12), upper bracket is movably installed on vacuum chamber body sidewall.
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| CN104889348B (en) * | 2015-06-19 | 2017-03-01 | 东方电气集团东方汽轮机有限公司 | The method of measurement high temperature alloy critical nuclei degree of supercooling |
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| CN100370591C (en) * | 2004-11-29 | 2008-02-20 | 吉林大学 | Forecasting method of single crystal internal connecting line-shaped nucleus and growth temp. |
| CN101279371A (en) * | 2007-12-28 | 2008-10-08 | 天津大学 | Method and device for preparing micro-uniform grain using harmonic method |
| CN101430292B (en) * | 2008-12-04 | 2011-05-04 | 上海大学 | Method for single metal droplet supercooling degree measurement by large cooling speed in situ fast thermal analysis |
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