CN1058536C - Ground simulation method and experiment equipment for spatial fast solidification - Google Patents
Ground simulation method and experiment equipment for spatial fast solidification Download PDFInfo
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- 238000002474 experimental method Methods 0.000 title claims description 7
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Abstract
本发明涉及一种空间快速凝固地面模拟方法与实验装置。它以调频电磁悬浮和超高真空技术为必要条件，以液态金属实现深过冷为充分条件。通过气体冷却实现悬浮熔炼过程中的温度控制，运用外部籽晶诱导异质形核对快速凝固过程进行主动控制；采用红外检测方法测定深过冷熔体的表面张力和晶体生长速度，以悬浮量热法测定其比热；将深过冷与急冷两种技术相结合实现三维快速凝固，并把落管微重力凝固复合到以悬浮无容器处理为主特征的实验装置中。The invention relates to a space rapid solidification ground simulation method and an experimental device. It takes the frequency modulation electromagnetic levitation and ultra-high vacuum technology as the necessary condition, and the liquid metal realizes the deep subcooling as the sufficient condition. The temperature control in the suspension smelting process is realized by gas cooling, and the rapid solidification process is actively controlled by using external seed crystals to induce heterogeneous nucleation; the surface tension and crystal growth rate of the deep supercooled melt are measured by infrared detection methods, and the suspension calorimetry The specific heat is determined by the method; the two technologies of deep subcooling and rapid cooling are combined to realize three-dimensional rapid solidification, and the microgravity solidification of the drop tube is combined into the experimental device characterized by suspension and container-free processing.
Description
The present invention relates to a kind of in ground environment the simulation liquid metal the spatial fast solidification process and it is carried out the method and apparatus of dynamic measurement and control.
In disclosed document, the Manifold technology that falls of frequency modulation electromagnetic suspension smelting technique is the present main method of virtual space material preparation process in ground environment, and " a kind of device of measuring supercooled liquid specific heat " (Apparafus tor the specificheatmeasurement of undercooled liquids) of report discloses a kind of will fall pipe and electromagnetic suspension and combine and realize the method for mensuration specific heat of liquid behind the high undercooling and discussed the feasibility of utilizing the electromagnetic suspension method can realize the high undercooling of large volume aluminium sample in U.S.'s metal digest 1991.6.But simultaneously, also point out in this document: because the error that fluctuating caused of suspended substance sample makes that the temperature measurement accuracy of pyrometer is very low.In the test that utilizes existing testing apparatus virtual space material rapid solidification, mainly there is following several respects deficiency in present test method and the testing installation:
1. difficult control of temperature in the frequency modulation electromagnetic suspension fusion process often causes the unstability that suspends when adopting gas cooling;
2. rapid solidification lacks ACTIVE CONTROL;
3. quick crystalline growth velocity measuring method complexity, and cost height;
4. be difficult to determine simultaneously the surface tension and the specific heat of high undercooling liquid metal;
5. only have simple function, can not be compound to multiple dynamic test in the experimentation with different rapid solidification modes.
" thermodynamic driving force of FORCE FOR RAPID CRYSTALLIZATION OF LIQUID METALS " of " Acta Metallurgica Sinica " Vol.30 No.7p289-293 report discloses a kind of employing ultrahigh vacuum(HHV) not to be had container suspended smelting technology and makes liquid Fe and Ni reach high undercooling and determine its specific heat by calorimetry, the method acquisition of high undercooling is to utilize melten glass preliminary cleaning---cyclical superheating processings---hydrogen reducing; And " metallurgical material " 1991, Vol.39No.6p1249-1258 discloses a kind of " high undercooling rapid solidification Ni-32.5%Si eutectic alloy ", and (HighUndercooling and Rapid Solidification of Ni-32.5%Si Eutectic Alloy) then discloses a kind of molten glass purification agent.These prior aries this paper is all in conjunction with reference.
The objective of the invention is, on an equipment, finish making suspended substance not unstability and energy ACTIVE CONTROL rapid solidification simultaneously when gas cooling, with lower cost, high temperature measurement accuracy is measured the surface tension and the specific heat of the crystalline speed of growth, high undercooling liquid metal simultaneously.
Technical solution of the present invention is, make liquid Fe and Ni supercooled spatial fast solidification method with electromagnetic suspension of no container frequency modulation and ultra high vacuum technique, it is characterized in that, the metal style is placed on the seed crystal, seed crystal is placed on the quartzy support tube of seed applying mechanism, connect high frequency electric source and realize specimen suspension, the heterogeneous nucleus of eliminating in the liquid metal under no container state makes melt reach high undercooling; Realize three-dimensional rapid solidification under the cooling conditions at a slow speed through the gas cooling of liquid nitrogen refrigerating; Use outside seed crystal to induce heterogeneous nucleus that sample is applied ACTIVE CONTROL.Present method with a kind of mainly by supervacuum chamber, detection system, gas system, sample control and seed applying mechanism, electromagnetic shutter thermal radiation resistant temperature lifting type suspension calorimeter, infrared quick crystalline growth velocity determinator, infrared suspended liquid drop surface oscillation detector, the liquid metal testing apparatus that pipe experiment mechanism and electromagnetic drive concave surface double-piston chilling mechanism form that atomizes, be under the prerequisite with high-frequency electromagnetic suspension and ultra high vacuum technique, with the Ni base, the Fe base, the Co base, Cu base or Ag base alloy style are placed on the seed crystal, seed crystal is placed on the quartzy support tube of seed applying mechanism, connect high frequency electric source and realize specimen suspension, the heterogeneous nucleus of eliminating under no container state in the liquid metal makes melt reach high undercooling, and the method acquisition of high undercooling is to utilize melten glass preliminary cleaning---cyclical superheating processings---hydrogen reducing; Realize three-dimensional rapid solidification under the cooling conditions at a slow speed through the gas cooling of liquid nitrogen refrigerating; Use outside seed crystal to induce heterogeneous forming core that sample is applied ACTIVE CONTROL; Adopt infrared detection method to measure the surface tension (σ L) and the crystalline growth velocity (V) of high undercooling melt simultaneously, measure its specific heat (CPL) with the suspension calorimetry; And will fall to managing microgravity solidify with two kinds of function compatibilities of chilling rapid solidification to being treated in the experimental installation of main feature with the no container that suspends.
Advantage of the present invention is, the spatial fast solidification process of simulation liquid metal in ground environment, and it is carried out dynamic measurement and control, the method of utilizing melten glass preliminary cleaning, cyclical superheating processing and hydrogen reducing to combine makes liquid metal be issued to deep cooling at suspended state, under the prerequisite of not destroying suspension stability the liquid metal that is suspending is implemented cooling and temperature control; Do the mensuration of surface tension (σ L) and specific heat (CPL) and crystalline growth velocity (V) simultaneously at the high undercooling liquid metal that dynamically is in suspended state down.The present invention also is being provided with a liquid metal atomising mechanism as suspend no container processing and supervacuum chamber top, thereby make experimental installation have the pipe of falling function, its effective free height of fall only is 0.5m, and droplet dia is 20～500 μ m, microgravity time 0.3s.It then is another significant feature of the present invention that high undercooling is combined with chilling, utilizes the concave surface double-piston chilling mechanism of electromagnetic drive to realize the rapid solidification of three-dimensional large volume liquid metal effectively.
Fig. 1 is the synoptic diagram of experimental installation of the present invention;
Experimental installation of the present invention mainly comprises supervacuum chamber 1, ultrahigh vacuum(HHV) obtains and detection system 2, suspended smelting coil 3, high-frequency induction heating power 4, test button 5, the liquid nitrogen refrigerating ring type six orifice gas cooling systems 6 that distribute, NdFeB permanent magnetism transmission Γ shape guide slot sample control and seed applying mechanism 7 (these parts separate case application, application number is 96114008.9), the pre-temperature lifting type suspension of electromagnetic shutter radioprotective calorimeter 8, infrared quick crystalline growth velocity determinator 9, infrared suspended liquid drop surface oscillation detector 10, CCD shooting and image analysis system 11, spectroscope 12, liquid metal atomizing and the pipe experiment mechanism 13 that falls, electromagnetic drive concave surface double-piston chilling mechanism 14, infrared temperature is measured and register system 15, general control system 16 and data collection and analysis system 17.
Dynamic operation mode is divided three kinds of situations:
1. heat determination is measured → compared to high undercooling → measurement of surface tension → rapid solidification → crystal growth rate;
2. high undercooling → measurement of surface tension → rapid solidification → crystal growth rate mensuration → chilling;
3. the liquid metal tubular type microgravity rapid solidification that atomizes → fall;
Method and apparatus of the present invention can be finished following function:
1. under the spatial simulation condition, make liquid metal obtain high undercooling;
2. study the crystal nucleation process in the high undercooling melt;
3. study the spatial fast solidification process;
4. measure high undercooling growth in melt speed;
5. measure the specific heat of high undercooling melt;
6. measure the surface tension of high undercooling melt;
7. the experiment of the pipe microgravity that falls rapid solidification;
8. realize three-dimensional rapid solidification with high undercooling with the chilling mode of combining;
9. the repertoire of compatible common suspended smelting and hammer anvil chilling quick solidification apparatus.
The present invention utilizes the molten glass purification agent to handle to test button preliminary cleaning and with cyclical superheating and the combine method of acquisition high undercooling of hydrogen reducing is: with analytical pure Na
2SiO
3, Na
2B
4O
7And B
2O
3The dehydration back fuses into 70%Na under 900～1200 ℃ of temperature respectively
2SiO
3+ 17.7%Na
2B
4O
7+ 12.3%B
2O
3The special glass scavenging agent.Glass melt, solidifies with stove then and is cooled to room temperature with abundant dehydration and degasification at 1000 ℃ of insulation 9～12h.This glass can be used as the scavenging agent of Ni base, Fe base, Co base, Cu base or Ag base alloy to eliminate heterogeneous nucleus.So-called " melten glass preliminary cleaning " is meant test button and 3～10g scavenging agent is placed silica tube, and induction heating to metal and scavenging agent all melts.At this moment, liquid metal is immersed among the melten glass.Under 100～300 ℃ of superheating temperature, Na under viscosity adsorption by melten glass and the high temperature
2B
4O
7And B
2O
3To the solubilizing reaction of metal oxide, can eliminate the purpose that heterogeneous nucleus reaches purification.Under the spatial simulation condition, the test button that purified is in advance carried out " fusing---solidify " with 100～500 ℃ of superheating temperature circulations handle, remaining heterogeneous nucleus is further fused.At last, in supervacuum chamber, feed the He-20%H of 10000～20000Pa
2Extraordinary mixed gas can make under the suspended state the lip-deep oxide compound of liquid metal be eliminated by hydrogen reducing.Liquid metal can obtain 0～500K condensate depression through eliminating after heterogeneous nucleus is handled.
The spatial fast solidification ground simulation experimental installation that the experimental installation of enforcement present method is made up of supervacuum chamber and detection system, suspended smelting coil is characterized in that the main composition of experimental installation is:
A. the handle that contains inside and outside permanent magnet in permanent magnetism transmission sample control and the seed applying mechanism is placed in the top of supervacuum chamber by bearing sleeve, the part of screw mandrel stretches into supervacuum chamber and silica tube and seed crystal is sent in the suspended smelting coil, rotary handle can make silica tube and seed crystal motion, and the high undercooling melt is applied outside seed crystal;
B. six nozzles of the ring type in the cooling system are arranged in supervacuum chamber, are connected by the liquid nitrogen refrigerating gas transfer pipeline of flange with the outside, and the gas of liquid nitrogen refrigerating is implemented cooling by six equally distributed nozzles to the drop of suspended state;
C. the pre-temperature lifting type suspension of electromagnetic shutter thermal radiation resistant calorimeter is arranged in supervacuum chamber, and its electromagnetic shutter is normally off and the control of controlled system between hanging drop and heat insulating sleeve, and the red copper piece is heated above a steady temperature of room temperature in advance.
Major parts 1 of the present invention, ring type six nozzles 6 place ultrahigh vacuum(HHV) indoor in the cooling system, connect by flange and outside gas storage bag 18 and source of the gas 21, effectively cool off to realize temperature control and rapid solidification through the liquid metal of liquid nitrogen refrigerating container 20 refrigerating gases suspended state, because six nozzles are evenly jet to exemplar, thereby can not destroy suspension stability.Pipeline beyond 19 pairs of vacuum chambers of vacuum pump 1 vacuumizes.
Major parts 3 of the present invention, the pre-temperature lifting type suspension of electromagnetic shutter thermal radiation resistant calorimeter 8 mainly comprise electromagnetic shutter 25, outward twine the red copper piece 26 that adds thermal resistance wire, twine the compositions such as heat insulating sleeve 27 that add thermal resistance wire outward, it places supervacuum chamber, and be connected with Controlling System 16, thermal radiation influence in the no container treating processes effectively prevents to suspend, and, make initial temperature drift not occur by in advance copper billet being heated above a certain steady temperature of room temperature.
Major parts 4 of the present invention, infrared quick crystalline growth velocity determinator 9 mainly comprises a big area high speed infrared diode and quartzy convex lens, it places a side of supervacuum chamber, whole sample is projected on the big area infrared diode, determine its recalescence time by instantaneous state recorder, then specimen size is exactly a crystalline growth velocity with the ratio of recalescence time.
Testing apparatus of the present invention is not only applicable to high-frequency electromagnetic suspended smelting technology, is applicable to the freely falling body to be the Manifold technology that falls of feature yet.It is realized by following method:
At the other inflation inlet (when doing high-frequency electromagnetic suspended smelting, this mouthful shut) that is provided with of the thermometric viewing window at supervacuum chamber top, when doing drop tube test, suspended coil and ring type nozzle are taken out, be replaced into the liquid metal pipe experiment mechanism 13 that atomizes.The liquid metal pipe experiment mechanism that atomizes is by set nut, the silica tube of band nozzle is formed, suspended coil in the vacuum chamber is replaced into common induction melting coil, and replace the cooling of ring type six orifice gases with ultrasonic atomizer, the air pressure that it is P1 that the vacuum chamber top charges into a pressure, the air pressure that it is P2 that ultrasonic atomizer charges into a pressure, when the gas stream of P2 pressure during through the ultrasonic atomizer nozzle, its flow velocity heightens, after charging into gas Ar, make the liquid metal that oozes in its silica tube be atomized into the fine droplet that diameter is 20～500 μ m, effectively height of fall is 0.5m, its rapid solidification under freely falling body microgravity condition in short-term of research in the time of 0.3s.
Another feature of the present invention is presented as on an equipment can not only finish high-frequency electromagnetic suspended smelting, the Manifold technology and high undercooling and two kinds of technology of chilling can being combined of falling, and eliminates solidification stages at a slow speed, more effectively realizes three-dimensional rapid solidification.Set up electromagnetic shutter radioprotective in the vacuum chamber that the swaps out suspension calorimeter that heats up in advance with electromagnetic drive concave surface piston Chiller, fall the moment of process silion cell detector when liquid metal, the silion cell signal makes pilot circuit work, drive bi-concave red copper chilling piston head and move simultaneously, thereby the liquid metal of high undercooling is clamped and chilling by piston head when falling into the two-piston head.For this reason, the electromagnetic drive concave surface double-piston chilling mechanism 14 among the present invention has finished this task.Electromagnetic drive concave surface double-piston chilling mechanism 14 is made up of concave surface red copper chilling piston head 28, no iron core electromagnetic drive coil 29, soft magnetic materials the axis of the piston and end cap 30, Si photocell detectors 31, rectifying circuit etc.During as high undercooling and the test of chilling rapid solidification, the pre-temperature lifting type suspension of electromagnetic shutter radioprotective calorimeter 8 in the vacuum chamber is replaced into electromagnetic drive concave surface double-piston chilling mechanism 14, when sample falls through Si photocell detectors 31, rectifying circuit work, no iron core electromagnetic drive coil 29 drives soft magnetic materials the axis of the piston and end cap 30, fall into the snap action of concave surface red copper chilling piston head 28 at drop, to reach the purpose that high undercooling combines with the chilling rapid solidification.
Embodiment:
Will be through the test button 5 usefulness sample controls and the seed applying mechanism 7 of purifying treatment are put into suspended coil 3 in advance.Take out ultrahigh vacuum(HHV) to predetermined vacuum level, anti-Ar or the He gas that fills certain pressure is driven high frequency electric source and is implemented suspended smelting.With infrared temperature measurement system 15 test samples temperature.But carry out temperature control by He or Ar air cooling.Adopt cyclical superheating and He-(15～25) %H
2The measure that cooling combines obtains high undercooling.Under certain condensate depression, measure the specimen surface oscillation frequency, thereby obtain its surface tension.As not having outside seed crystal, free rapid solidification will take place in the high undercooling melt.Apply its rapid solidification under predetermined condensate depression of outside seed crystal may command.Two kinds of situations all can be measured the crystalline growth velocity under the corresponding condensate depression.Under certain condensate depression, the high undercooling melt is splashed into suspension calorimeter 8, measure its specific heat.As with concave surface double-piston chilling mechanism 14 displacement suspension calorimeters 8, realize that then high undercooling combines with the chilling rapid solidification.Replace suspended coil 3 and atomising mechanism 13 is installed, the pipe microgravity that can fall rapid solidification with common load coil.
Claims (7)
1. make liquid Fe and Ni supercooled spatial fast solidification method with electromagnetic suspension of no container frequency modulation and ultra high vacuum technique, it is characterized in that, the metal style is placed on the seed crystal, seed crystal is placed on the quartzy support tube of seed applying mechanism, connect high frequency electric source and realize specimen suspension, the heterogeneous nucleus of eliminating in the liquid metal under no container state makes melt reach high undercooling; Realize three-dimensional rapid solidification under the cooling conditions at a slow speed through the gas cooling of liquid nitrogen refrigerating; Use outside seed crystal to induce heterogeneous nucleus that sample is applied ACTIVE CONTROL.
2. the method for spatial fast solidification method according to claim 1 is characterized in that, high undercooling is to utilize melten glass preliminary cleaning---cyclical superheating processing---hydrogen reducing obtains.
3. according to claim 1 or described spatial fast solidification method, it is characterized in that, set up electromagnetic shutter radioprotective in the vacuum chamber that the swaps out suspension calorimeter that heats up in advance with electromagnetic drive concave surface piston Chiller, fall the moment of process silion cell detector when liquid metal, the silion cell signal makes pilot circuit work, drive bi-concave red copper chilling piston head and move simultaneously, thereby the liquid metal of high undercooling is clamped and chilling by piston head when falling into the two-piston head.
4. spatial fast solidification ground simulation experimental installation of implementing claim 1 is characterized in that the main composition of experimental installation is:
A. the handle that contains inside and outside permanent magnet in permanent magnetism transmission sample control and the seed applying mechanism is placed in the top of supervacuum chamber by bearing sleeve, the part of screw mandrel stretches into supervacuum chamber and silica tube and seed crystal is sent in the suspended smelting coil, rotary handle can make silica tube and seed crystal motion, and the high undercooling melt is applied outside seed crystal;
B. six nozzles of the ring type in the cooling system are arranged in supervacuum chamber, are connected by the liquid nitrogen refrigerating gas transfer pipeline of flange with the outside, and the gas of liquid nitrogen refrigerating is implemented cooling by six equally distributed nozzles to the drop of suspended state;
C. the pre-temperature lifting type suspension of electromagnetic shutter thermal radiation resistant calorimeter is arranged in supervacuum chamber, and its electromagnetic shutter is normally off and the control of controlled system between hanging drop and heat insulating sleeve, and the red copper piece is heated above a steady temperature of room temperature in advance.
5. spatial fast solidification ground simulation experimental installation according to claim 4, it is characterized in that, the infrared quick crystalline growth velocity determinator of detection system is positioned at the side of supervacuum chamber, aims at the sample in the vacuum chamber and whole sample is projected on the big area infrared diode.
6. spatial fast solidification ground simulation experimental installation according to claim 4, it is characterized in that, replace ring type six nozzles with ultrasonic atomizer, and be fixed in upper top in the vacuum chamber, replace the suspended smelting coil with common induction melting coil, the liquid metal atomizing that charges into refrigerant gas and ooze in silica tube through ultrasonic atomizer.
7. spatial fast solidification ground simulation experimental installation according to claim 4 is characterized in that, the virtual height that liquid metal falls in the pipe experiment mechanism silica tube that falls is 0.5m.
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|---|---|---|---|
| CN96114009A CN1058536C (en) | 1996-12-27 | 1996-12-27 | Ground simulation method and experiment equipment for spatial fast solidification |
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|---|---|---|---|
| CN96114009A CN1058536C (en) | 1996-12-27 | 1996-12-27 | Ground simulation method and experiment equipment for spatial fast solidification |
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| CN1158916A CN1158916A (en) | 1997-09-10 |
| CN1058536C true CN1058536C (en) | 2000-11-15 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4377375A (en) * | 1981-03-02 | 1983-03-22 | United Technologies Corporation | Apparatus for forming alloy powders through solid particle quenching |
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1996
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4377375A (en) * | 1981-03-02 | 1983-03-22 | United Technologies Corporation | Apparatus for forming alloy powders through solid particle quenching |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1306275C (en) * | 2003-08-01 | 2007-03-21 | 中国科学院金属研究所 | Transparent down pipe for analogue micro gravity experiment |
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| CN1158916A (en) | 1997-09-10 |
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