CN104588622B - Metal bath bulk nanostructured material preparation system - Google Patents
Metal bath bulk nanostructured material preparation system Download PDFInfo
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- CN104588622B CN104588622B CN201410816445.7A CN201410816445A CN104588622B CN 104588622 B CN104588622 B CN 104588622B CN 201410816445 A CN201410816445 A CN 201410816445A CN 104588622 B CN104588622 B CN 104588622B
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- vacuum chamber
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- metal bath
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/02—Use of electric or magnetic effects
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/04—Influencing the temperature of the metal, e.g. by heating or cooling the mould
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/15—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting by using vacuum
Abstract
The present invention relates to metal bath bulk nanostructured material preparation system, the structure of the system is as follows：Mechanical pump (1) to be connected with molecular pump (2) and be connected to flapper valve (4) with flange；Flapper valve (4) is while with screwed connection angle valve (3), another side flange is connected to vacuum chamber components (5)；Electromagnet (6) is shelved by equipment board (8) on the both sides of vacuum chamber components, upper lid lifting assembly (7) is connected on equipment board (8) by flange to be used to lift by crane on vacuum chamber lid (16), to feed, discharging；In vacuum chamber cavity (10), Pirani gauge (9), ionization gauge (11), DC pulse electrode (12), sensing heating electrode (13), infrared measurement of temperature window (14), thermocouple temperature measurement electrode (15), load coil (19) are respectively mounted by welding；An intake valve (17) is connected by flange in the another side of vacuum chamber cavity (10) and is provided with the ceramic crucible (18) being connected with support by bolt for leading to inert gas shielding, inside.
Description
Technical field
The system is the horizontal high vacuum supercooling metal bath bulk nanostructured material preparation system with water-cooled nested structure of single chamber,
Can be used to develop the research of nano level metal alloy compositions and preparation etc..
Background technology
Under current experiment condition, in addition to a small number of alloy systems are more than cold rapid solidification, for Practical Project material, no matter
It is the high undercooling rapid solidification for reaching critical undercooling limits Δ T*, or the curing condition such as pulse current and Microgravity effect
Under, all it is difficult to the grain size of material is reached nanometer scale by its single refining effect.
The content of the invention
The present invention relates to a kind of metal bath bulk nanostructured material preparation system, can be in simulated microgravity+electric pulse+depth
Bulk nanostructured material equipment is prepared under three kinds of collective effects of mechanism of supercooling, it is also possible to which a certain mechanism is used alone carries out material
Preparation research.
First, electromagnetical analogies microgravity principle
Under the conditions of common ground, due to gravity influence, phase separation is also easy to produce during solidification.Sample in process of setting, due to
Influenceed by the Stokes sedimentary effects that gravity is produced, two constituent elements with unmixability gap are layered in state is kept completely separate
Phenomenon clearly, with the naked eye can also observe directly a small number of profiles for matrix separate.A small number of phase contents must be typically controlled,
It is general to take the measures such as Quench, stirring or addition alloying element to eliminate segregation.
If as shown in figure 1, metal bath is positioned in the electric field and magnetic field for being mutually perpendicular to intersect, excited in a liquid
Electromagnetism volume power will act in each unit volume of material, its physical property is similar to gravity.Given in magnetic induction density B
In the case of fixed, can be by constantly regulate current density, J0Size makes the effective gravity of dispersoid and matrix equal, so that whole
Individual melt is under quasi- state of weightlessness all the time, here it is the effect of electromagnetical analogies microgravity.
Existing research shows：
1st, under the usual terms of ground, the Stokes sedimentary effects that gravity causes cause metal alloy to be separated
Main cause, it is acted on considerably beyond other mechanism.
2nd, microgravity electromagnetic analogue can effectively eliminate Stokes sedimentary effect of the alloy in process of setting, profit
The mixed alloy sample of the good difficulty of disperse structure can be successfully prepared with the device.
3rd, determine that a good and bad key factor of difficult mixed alloy property is the size of a small number of phases and its in matrix (most phases)
In distribution situation.A small number of phase sizes are smaller, it is more uniform to be distributed, and the performance of material is better.
2nd, electric pulse action principle (as shown in Figure 2)
By research, influence of the pulse current to nucleation rate is mainly and is changed degree of supercooling and realized by it.Classical forming core
Theory lists nucleation rate expression formula：
In formula, I is nucleation rate, and h is Planck's constant, and n is unit volume atomicity, and K is Boltzmann constant, and T is exhausted
To temperature, σs1It is unit surface free energy, TmIt is fusing point, Δ T=Tm- T is the degree of supercooling of melt, LmIt is the latent heat of fusion, Δ GAFor
Liquid atomic nucleating potential barrier.
By formula (1-1) it is seen that, if improve melt degree of supercooling and reduce liquid atomic nucleating potential barrier if shape
Core rate will be enhanced, thus for nanocrystalline realization is laid a good foundation.As shown in Fig. 2 we are electric to analyze pulse below
Such effect can be realized after field action melt.
Axial symmetry electric currentMagnetic field is produced by cylindrical conductive meltIt is assumed that pulse current is logical
Produced electromagnetic force and the aspect of Joule heat two is crossed to influence degree of supercooling.Providing the lower degree of supercooling relational expression of pulse current effect is：
In formula, Δ T0Degree of supercooling when being without current pulse；ΔTP=αPIt is that electromagnetic force is led under pulse current effect
The increase of the degree of supercooling of causeA is the radius of cylindrical melt, and r is in melt
Distance of any point to central axis)；It is that (R is conductor resistance, t to the thermogenetic degree of supercooling of joule
It it is pulse current action time, m is workpiece quality, and C is specific heat)；K=R/mC.
Analytical formula (1-2) understands, if in the case that the Joule heat very little of impulse electric field generation is so that ignore, melted
The degree of supercooling of body can just be increased.Derive in theory when there is pulse current, pulse width meets τ ∝ K1·|ξ|·
V·σ0·ρ·λ·k-1Under the conditions of, electric current not only to produce joule heat affecting very little so that can be ignored, Er Qie electricity
The change of the nucleating potential barrier that the contribution of field can also cause, i.e.,：The Δ G in former nucleation rate equation (1-1)AΔ G will be changed intoA=Δ
G0+ΔGEThis, Δ G0Forming core thermodynamics potential barrier when being without outfield, Δ GEThere is forming core thermodynamic potential during outer field action
Build, i.e.,：
ΔGA=(Δ G0+ΔGE)=Δ G0+K1·j2·ζ2·V (1-3)
Wherein, ξ=(σ0-σn).(σn-2σ0)-1
K1The parameter related to material, j pulse current densities, σ0The conductance of Disordered Media, σnThe electrical conductivity of nucleus, V is brilliant
The volume of core, k Boltzmann constants.
The σ for melt crystallizationn＞ σ0, then ξ ＞ 0, it is seen that K1·j2·ξ2V ＜ 0, this demonstrate pulse current reduction
Nucleating potential barrier, such analysis equation (1) understands that nucleation rate ratio does not have pulse current to be increased in the case of acting on.According to
Avrmai equations, the increase of nucleation rate will cause the refinement of crystal grain.
Knowable to above-mentioned theory analysis, after high impulse electric field acts on subcooling films, the supercooling of melt is not only increased
Degree, and the nucleating potential barrier of melt is reduced, forming core is greatly improved, such coupling mechanism is conducive to the refinement of nucleus,
Also it is to realize that bulk nanostructured material is laid a good foundation.
3rd, high undercooling action principle
The degree of supercooling of metal bath refers to equilibrium freezing temperature TLWith actual nucleation temperature TNDifference.By to liquid metal
The research of high undercooling can reveal that the nucleation mode of process of setting, calculate the unknown thermal physical property parameter in part, prediction heterogeneous nuclei
Nucleation ability, checking rapid solidification is theoretical and prepares block rapid solidification new material etc..Materials microstructure determines its property
Can, the final form of solidified structure depends on the evolutionary process that early solidification mutually selected and solidify later stage tissue, and these processes
Degree of supercooling mostly with metal bath is directly related.Therefore, high undercooling is exactly to make metal bath reach the degree of supercooling limit to be coagulated
Solid method.
Under normal circumstances, the solidification of metal bath is carried out by heterogeneous nucleation mode.It is deep to obtain liquid metal
Supercooling must be purified to it, eliminate or be passivated the heterogeneous nuclei in melt.Generally, the method for obtaining thermodynamics high undercooling has：(a)
Fine droplet method, (b) emulsification-thermal analysis system, (c) cyclical superheating method, (d) molten glass purification method, (e) electromagnetic levitation-melt
Method, (f) fall tube method etc..
The present invention relates to metal bath bulk nanostructured material preparation system, the system includes following equipment：It is electromagnet, true
Empty room, sensing heater, magnet power supply, DC current power supply, vacuum and protective gas inflation system, temperature and true
Empty measurement, control system, data acquisition, storage, treatment, display and output system.
Brief description of the drawings
Be more fully described exemplary embodiment of the invention by referring to accompanying drawing, above and other aspect of the invention and
Advantage will become more easily clear, in the accompanying drawings：
Fig. 1 is electromagnetical analogies microgravity principle schematic；
Fig. 2 is electric pulse action principle schematic diagram；
Fig. 3 is the first sectional view of metal bath bulk nanostructured material preparation system of the invention；
Fig. 4 is the second sectional view of metal bath bulk nanostructured material preparation system of the invention；
Fig. 5 is the top view of metal bath bulk nanostructured material preparation system of the invention；
Fig. 6 is the side view of metal bath bulk nanostructured material preparation system of the invention；
Fig. 7 is the front view of metal bath bulk nanostructured material preparation system of the invention.
Specific embodiment
Hereinafter, the present invention is more fully described now with reference to accompanying drawing, various embodiments is shown in the drawings.So
And, the present invention can be implemented in many different forms, and should not be construed as limited to embodiment set forth herein.Phase
Instead, there is provided these embodiments cause that the disclosure will be thorough and complete, and fully convey the scope of the present invention to ability
Field technique personnel.
Hereinafter, exemplary embodiment of the invention is more fully described with reference to the accompanying drawings.
As shown in Figure 3, Figure 4, reference implication and effect are as follows：
1- mechanical pumps：Fore pump, takes out black vacuum
2- molecular pumps：Master takes out pump, takes out end vacuum
3- angle valves：The switch of mechanical pump and vacuum chamber
4- flapper valves：Realize the switch of molecular pump and vacuum chamber
5- vacuum chamber components：The component of vacuum chamber working chamber composition
6- electromagnet：After energization, the transverse magnetic field of vertical sample is produced
The upper lid lifting assemblies of 7-：After releasing vacuum, covered on lifting vacuum chamber
8- equipment boards：The board of the parts such as place apparatus, magnet and power supply
9- Pirani gauges：Measurement rough vacuum
10- vacuum chamber cavitys：Working cavity
11- ionization gauges：Measurement high vacuum
12- DC pulse electrodes：DC pulse current is applied to sample
13- sensing heating electrodes：For being powered to induction coil, sensing heating
14- infrared measurement of temperature windows：Infrared radiation thermometer is installed, sample temperature is measured
15- thermocouple temperature measurement electrodes：Connection tungsten-rhenium wire, thermocouple temperature measurement
Covered on 16- vacuum chambers：For driving vacuum chamber and fixed electrode, induction coil, crucible etc.
17- intake valves：Working gas is passed through by intake valve
18- ceramic crucibles：For holding sample
19- load coils：Connect 13 sensing heating electrodes, sensing heating after energization.
Wherein, flapper valve 4 is connected to after mechanical pump 1 is connected with molecular pump 2 with flange；One side of flapper valve 4 is connected with screw thread
Angle valve 3 is connect, another side flange is connected to vacuum chamber components 5.Electromagnetism is shelved by equipment board 8 on the both sides of vacuum chamber components
Iron 6, upper lid lifting assembly 7 is connected on equipment board 8 by flange to be used to lift by crane lid 16 on vacuum chamber, to feed, discharging.
In vacuum chamber cavity 10, Pirani gauge 9, ionization gauge 11, DC pulse electrode 12, sensing are respectively mounted by welding
Heating electrode 13, infrared measurement of temperature window 14, thermocouple temperature measurement electrode 15, load coil 19；In the another of vacuum chamber cavity 10
Side connects an intake valve 17 by flange to be used to lead to inert gas shielding, and inside is provided with the ceramics being connected with support by bolt
Crucible 18.
The course of work of the invention is as follows：
1. lid on vacuum chamber 16 is lifted by upper lid lifting assembly 7, installs former equipped with experiment in vacuum chamber cavity 10
The ceramic crucible 18 of material, fills a certain amount of B in experimental raw2O3, increase the degree of supercooling of melt, i.e., high undercooling is applied to melt
Mechanism, then installs lid 16 on vacuum chamber；
2. open mechanical pump 1 to be evacuated down to less than 10Pa, be then turned on molecular pump 2 and be evacuated down to 1 × 10-5Pa；
3. turn on the power switch after carrying out being heated to uniform temperature to experimental raw with load coil 19, close heating
Power supply, unlatching intake valve 17 leads to inert gas to be protected；
4. it is then turned on heating power supply and is heated up to more than the fusing point of experimental raw 50~100 DEG C being incubated；
5. heating power supply is closed, electromagnet 6 and direct current pulse power source 12 is opened and is applied microgravity and electric arteries and veins respectively to melt
Punching is acted on；
6. after after melt solidification, electromagnet 16 and direct current pulse power source 12 are closed, after being cooled to room temperature, opens angle valve 3 and put
Fall vacuum and inert protective gas, open lid 16 on vacuum chamber and take out experimental raw.
The electromagnet determines according to the parameter request of system；Pole dimension is about between >=200mm × 150mm, magnetic pole
The continuously adjustable between from 60mm to 170mm.During maximum magnetic flux die opening, magnetic induction density B=0.5T. is in effective test block
Magnetic field inhomogeneity degree is less than 2.7%, and the effective coverage in magnetic field is 200X50mm.
Magnetic Circuit Design parameter is as follows；
Coil cold-state resistance：R=0.35 Ω
Coil current：I=40A
Coil voltage：V=150V
Magnetic pole area：200mm×150mm
Coil power；P=IV=6Kw；
Electromagnetism weight of iron W=1900Kg
Coil allows temperature rise：80℃.
To reduce coil temperature rise, originally water cooling can be used, water-carrying capacity is 9 liters/min.
Electromagnet excitation magnetic power supplying power supply uses thyristor dc stabilized current supply, with reference to model KYA-50A/180V, electric current
Adjustable extent is 0~50A.Average temperature degree is better than 1%.
The main technical performance index of the vacuum chamber is as follows：
1. vacuum chamber structure and size
1.1 vacuum chambers：About 500 length × 160 width × 280mm a height of square shape vertical side's door additional water collars of full magnetism-free stainless steel
Structure.Above each with upper lid to fill a quartz observing window of Φ 63, valve is taken out on an air inlet stop valve a, side.Each flange seal
Mouth is outer using fluorine rubber ring sealing.
1.2 additional electromagnetic fields：In two sides of vacuum chamber added with the electromagnetic field perpendicular to crucible axial direction, magnetic induction intensity is most
It is about during big magnetic pole spacing：B=0.5T；Magnetic field inhomogeneity degree is less than 2.7% in effective test block.I.e.：Pole pitch body of heater
When in 30mm to 85mm adjustable extents, the center field intensity of its body of heater 170mm reaches 0.5 tesla, scope 200X50mm.
1.3 are furnished with load coil in vacuum chamber, and the crucible in coil is heated, and heating-up temperature is not less than
1200 DEG C,
1) Wolfram rhenium heat electric couple feedback observing and controlling temperature.Control temperature is better than ± 2.5 DEG C；
2) infrared radiation thermometer, calibrates thermometric.
The two of 1.4 crucibles are terminated with metal electrode, after sample heating meets heating-up temperature, can lead to after stopping sensing heating
Cross two termination electrodes and DC pulse voltage, electric current are applied to sample.
2. vacuum acquirement and measurement
2.1 the system are evacuated to vacuum chamber respectively using a set of FF100/110 types molecular pump+2XZ-4 mechanical pumps, are led to
Cross a Dg100 valves and realize that master takes out, bypass pumping is realized by a Dg35 angle valves.
2.2 system limits vacuum
Vacuum chamber：The toasted rear continuous air extraction of system, unloaded vacuum is up to 5 × 10-3Pa；Short time exposure air is simultaneously
It is filled with drying nitrogen and starts pumping, 40 minutes up to 6.6 × 10-4Pa.Vacuum system integral leakage is less than 1 × 10-4PaL/S.
2.3 vacuum measurements：Measured using the compound high vacuum gauge of a ZDF5227 digital display.
2.4 inflation systems：The system is by gas cylinder, pressure-reducing valve, regulating valve, mass flowmenter, pressure gauge and pipeline structure
Into.The use of gas is nitrogen and argon gas.
3. power supply
3.1st, sensing heating temperature-controlled power：It is a set of
3.1.1, power：30KW
3.1.2, frequency：40-80HZ
3.2nd, DC pulse extra electric field power supply
3.2.1, input voltage：220 or 380V is exchanged
3.2.2, pulse input power：Less than or equal to 25KW
3.2.3, current density：100A~10000A/cm2It is adjustable
3.2.4, pulse output frequencies：1Hz~1000Hz continuously adjustabes
3.2.5, pulse width：5 μ s~100 μ s continuously adjustabes
3.2.6, pulse current direction：Unidirectional or bidirectional output
3.2.7, the precision of voltage regulation：≤ 1%
3.3rd, master control power supply：1.
4th, air-channel system：
Using two road MFC mass flow meter controller air inlets, it are furnished with a Dg16 manual shutoffs before every mass flowmenter all the way
Valve.
5th, water-cooled and warning system：
System is furnished with water-cooled and water flow alarm system, for carrying out water cooling to molecular pump, magnet exciting coil, vacuum chamber etc.,
Water flow relay is installed on water route, once water shortage or hydraulic pressure are not enough, corresponding power supply will be alarmed and cut off, in case stopping loss
Bad equipment.
6th, computer control system：
The system can data acquisition, storage, treatment, display and output function.By the magnet power supply of whole system, direct current
The controls such as source, sensing heating, vacuum system, temperature survey, data acquisition, storage, treatment, display and output, are integrated in industry control
Machine or PC, constitute display panel.
Embodiments of the invention are the foregoing is only, is not intended to limit the invention.The present invention can have various conjunctions
Suitable change and change.All any modification, equivalent substitution and improvements made within the spirit and principles in the present invention etc., all should
It is included within protection scope of the present invention.
Claims (2)
1. metal bath bulk nanostructured material preparation system, it is characterised in that the structure of the system is as follows：
Mechanical pump (1) is connected to flapper valve (4) after being connected with molecular pump (2) with flange；One side screwed connection of flapper valve (4)
Angle valve (3), another side flange is connected to vacuum chamber components (5)；Shelved by equipment board (8) on the both sides of vacuum chamber components
Electromagnet (6), upper lid lifting assembly (7) is connected on equipment board (8) by flange is used to lift by crane lid (16) on vacuum chamber, with
Civilian dress material, discharging；
In vacuum chamber cavity (10), by welding be respectively mounted Pirani gauge (9), ionization gauge (11), DC pulse electrode (12),
Sensing heating electrode (13), infrared measurement of temperature window (14), thermocouple temperature measurement electrode (15), load coil (19)；In vacuum chamber
The another side of cavity (10) connects an intake valve (17) and is provided with by bolt for leading to inert gas shielding, inside by flange
The ceramic crucible (18) being connected with support；
Said system operation principle is as follows：
1. (16) will be covered on vacuum chamber to lift, installed equipped with experiment in vacuum chamber cavity (10) by upper lid lifting assembly (7)
The ceramic crucible (18) of raw material, then installs lid (16) on vacuum chamber；
2. open mechanical pump (1) to be evacuated down to less than 10Pa, be then turned on molecular pump (2) and be evacuated down to 1 × 10-5Pa；
3. turn on the power switch after carrying out being heated to uniform temperature to experimental raw with load coil (19), close heating electricity
Source, opens the logical inert gas of intake valve (17) and is protected；
4. it is then turned on heating power supply and is heated up to more than the fusing point of experimental raw 50~100 DEG C being incubated；
5. heating power supply is closed, electromagnet (6) and direct current pulse power source is opened and is applied microgravity and electric pulse work respectively to melt
With；
6. after to be solidified, electromagnet and direct current pulse power source are closed, after being cooled to room temperature, opens angle valve (3) and bleed off vacuum and lazy
Property protective gas, open vacuum chamber on lid (16) take out experimental raw.
2. metal bath bulk nanostructured material preparation system as claimed in claim 1, it is characterised in that in above-mentioned ceramic crucible
(18) B of increase melt undercooling degree is filled in the experimental raw of dress2O3。
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| CN109482847A (en) * | 2018-12-27 | 2019-03-19 | 江苏奇纳新材料科技有限公司 | Magnetic-moves the molding machine and method of combined precision complexity fine grain casting |
| CN110042327A (en) * | 2019-05-28 | 2019-07-23 | 北方民族大学 | A kind of a wide range of controllable Biological magnesium alloy of degradation rate |
| CN110541088B (en) * | 2019-09-06 | 2021-01-05 | 北方民族大学 | Method for improving microstructure of Cu-Pb hypermonotectic alloy |
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| CN1324159C (en) * | 2005-06-06 | 2007-07-04 | 辽宁工学院 | Method for preparing nanocystalline ingot casting by magnetic field and ultrasonic combined treatment of metal melt and dedicated apparatus therefor |
| CN2856060Y (en) * | 2005-10-11 | 2007-01-10 | 中国科学院物理研究所 | High vacuum in-situ refining equipment extracting high pure material |
| CN101418386B (en) * | 2007-10-26 | 2010-06-23 | 中国科学院金属研究所 | Equipment for preparing multifunctional amorphous composite material |
| CN101348903B (en) * | 2008-08-29 | 2011-12-28 | 中国石油大学(北京) | Multifunctional small film deposition equipment |
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