CN116140593A - Control method for solidification condition of electrostatic suspension alloy melt - Google Patents
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Abstract
The invention relates to a control method of static suspension alloy melt solidification conditions, which solves the problem that the alloy melt solidification conditions are difficult to control under the condition of static suspension without a container, and realizes the active control of alloy melt cooling rate and supercooling degree: (1) In the natural cooling process, the size of the alloy melt is reduced, so that the cooling rate of the alloy melt can be increased; during the cooling of the alloy melt, laser light is applied to reduce the cooling rate. Whereby solidification of the alloy melt under a variety of different cooling rate conditions can be controlled. (2) The control of the alloy melt temperature is realized by two methods of a heat balance equation and a PID temperature control system, and the active control of the solidification supercooling degree of the alloy melt is realized by combining triggering nucleation, so that the problem that the supercooling degree of the alloy melt is difficult to regulate randomly under the electrostatic suspension condition is solved.
Description
Technical Field
The invention belongs to the field of heat transfer and alloy solidification control of electrostatic suspension melt, relates to a control method of solidification conditions of electrostatic suspension alloy melt, and in particular relates to a method for adjusting and controlling cooling rate and supercooling degree of alloy melt under the condition of electrostatic suspension without a container.
Background
The electrostatic suspension technology has the advantages of no container, high vacuum, stable suspension, small disturbance of external field and the like, and becomes an important way for realizing suspension melting of alloy (particularly high temperature and refractory alloy) and realizing deep supercooling rapid solidification. However, in the electrostatic suspension experiment, the alloy melt in the high vacuum environment is only radiated to a deep supercooling state, and the cooling rate and supercooling degree of the alloy melt are difficult to effectively regulate. The solidification process of the alloy melt is closely related to the microstructure and mechanical properties of the alloy melt, and the control of the solidification conditions of the alloy melt under the static suspension condition, such as cooling rate and supercooling degree, is an important method for obtaining various solidification paths and microscopic phase compositions of the alloy, and is a necessary premise for realizing the control of the alloy solidification process and the regulation of the mechanical properties.
The key of regulating and controlling the solidification condition (cooling rate and supercooling degree) of the alloy melt under the electrostatic suspension condition is to clarify and control the heat transfer process of the alloy melt. "method for growing high-temperature and refractory alloy spherical single crystals under static conditions", CN 111020704a, hu Liang, wei Bingbo "relates to temperature control of alloy melt under static suspension conditions, but only refers qualitatively to the fact that alloy melt of different sizes can obtain different cooling rates under the action of different laser powers, lacks quantitative analysis of heat transfer process of alloy melt, and does not clarify control mechanism and method of cooling rate and supercooling degree thereof. The cooling rate of the melt can be varied but the main concern is to form spherical single crystals by means of an electrostatic suspension containment-free process, which allows high temperature and refractory alloy melts to reach a supercooling degree above the cold critical supercooling degree. "M.X.Li, H.P.Wang, wei. Numerical analysis and experimental verification for heat transfer process of electrostatically levitated alloy droplets, international Journal of Heat and Mass Transfer,2019,138:109-116," the heat transfer process of an electrostatically suspended alloy melt was analyzed numerically, but the information of temperature distribution, temperature gradient, cooling rate, etc. inside an alloy melt of any morphology was solved numerically by a finite volume method.
Under the static suspension condition, the alloy melt has single cooling rate under the natural radiation heat dissipation condition, and the solidification supercooling degree is randomly controlled, so that the solidification process of the alloy melt is difficult to effectively regulate and control. The existing experimental means and heat transfer analysis can not realize the active control of the solidification conditions (cooling rate and supercooling degree) of the alloy melt. The cooling rate is regulated and controlled by changing the size of the alloy melt and the laser power, and the active control of the supercooling degree of the alloy melt is realized by combining the melt temperature control and the triggering nucleation, so that the cooling rate and the supercooling degree of the static suspension alloy melt during solidification are effectively regulated and controlled, and the method has important significance for regulating and controlling the solidification process and the mechanical property of the alloy melt.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a control method for the solidification condition of an electrostatic suspension alloy melt, and aims at the limitation that the cooling rate of the alloy melt is single and the supercooling degree is difficult to regulate and control randomly under the electrostatic suspension condition.
Technical proposal
A control method of the solidification condition of an electrostatic suspension alloy melt is characterized in that: controlling the cooling rate and supercooling degree of the alloy melt under the condition of electrostatic suspension:
step 1: in an ultrahigh vacuum electrostatic suspension experimental device, a spherical alloy sample is stably suspended in a strong electric field between an upper electrode and a lower electrode, and the alloy sample is in a melting overheat state by laser heating;
wherein m, A, C P T and epsilon are the mass, surface area, specific heat, temperature and heat radiation coefficient of the alloy melt respectively; sigma is Stefan-Boltzmann constant; t (T) e Is the external environment temperature; p (P) E For an effective laser power applied to the melt surface;
left end of equationIndicating the temperature change of the alloy melt, radiating by radiation at the right end +.>And laser heating P E Determining the combined action;
cooling rate R c The method comprises the following steps:
the diameter D of the alloy melt is inversely proportional to the cooling rate, and the cooling rate is increased or decreased by reducing or increasing the diameter D of the alloy melt;
by controlling the effective laser power applied to the alloy melt surface to be P according to the heat balance equation E Maintaining it at a set temperature T set ;
Step 5: when the alloy melt is kept at the set temperature, the solidification of the alloy melt is realized, and the active control of the solidification supercooling degree of the alloy melt is realized.
The diameter of the spherical alloy sample is 1-6 mm.
The cooling rate is regulated and controlled in the step 3, and the cooling rate is regulated and controlled by changing the laser power; according to the cooling rateThe laser power is inversely proportional to the alloy melt cooling rate, and by decreasing or increasing the laser power, the cooling rate is increased or decreased accordingly.
The alloy melt temperature in the step 4 is controlled, when the alloy melt is cooled to the temperature control set temperature T set When the laser power is nearby, the PID temperature control system is used for adjusting the laser power:wherein k is P 、k I 、k D The laser power is regulated in real time according to the formula, so that the alloy melt is stably kept at the specified temperature.
Advantageous effects
The control method of the static suspension alloy melt solidification condition solves the problem that the alloy melt solidification condition is difficult to control under the static suspension container-free condition, and realizes the active control of the alloy melt cooling rate and supercooling degree: (1) In the natural cooling process, the size of the alloy melt is reduced, so that the cooling rate of the alloy melt can be increased; during the cooling of the alloy melt, laser light is applied to reduce the cooling rate. Whereby solidification of the alloy melt under a variety of different cooling rate conditions can be controlled. (2) The control of the alloy melt temperature is realized by two methods of a heat balance equation and a PID temperature control system, and the active control of the solidification supercooling degree of the alloy melt is realized by combining triggering nucleation, so that the problem that the supercooling degree of the alloy melt is difficult to regulate randomly under the electrostatic suspension condition is solved.
Drawings
FIG. 1 is a schematic diagram of a method for controlling solidification conditions of an electrostatically suspended alloy melt
FIG. 2 is a graph showing cooling curves of alloy melt under natural radiation heat dissipation
FIG. 3 is a graph showing cooling rate modulation achieved by varying the alloy melt size; (b) Cooling rate
FIG. 4 is a graph showing alloy melt cooling rate modulation by varying laser power (a) cooling profile; (b) Cooling rate
FIG. 5 is a graph of effective laser power for alloy melt supercooling control based on a thermal equilibrium equation; (b) Temperature control curve
FIG. 6 shows the realization of supercooling degree control of alloy melt based on PID temperature control system
FIG. 7 solidification of electrostatically suspended alloy melts at different degrees of supercooling
Detailed Description
The invention will now be further described with reference to examples, figures:
the invention provides a control method of static suspension alloy melt solidification conditions, which aims at the limitation that the alloy melt cooling rate is single and the supercooling degree is random and difficult to regulate and control under the static suspension conditions.
A control method of static suspension alloy melt solidification condition comprises the following steps of:
and step 1, in an ultrahigh vacuum electrostatic suspension experimental device, stably suspending a spherical alloy sample with the diameter of 1-6 mm in a strong electric field between an upper electrode and a lower electrode, and heating the alloy sample to a molten and overheated state by laser.
wherein m, A, C P T and epsilon are the mass, surface area, specific heat, temperature and heat radiation coefficient of the alloy melt respectively; sigma is Stefan-Boltzmann constant; t (T) e Is the external environment temperature; p (P) E For the effective laser power applied to the melt surface.
The left term of equation (1) represents the temperature change of the alloy melt, determined by the combined action of radiant heat dissipation (right first term) and laser heating (right second term).
Changing the size of the alloy melt:
in the natural cooling process, the right term P in the alloy melt temperature equation (1) E =0, rewritable as:
wherein D is the melt diameter. Cooling rate R c Can be expressed as:
from the formula (3), it is known that by decreasing the diameter of the alloy melt, the cooling rate thereof can be increased.
2. Adjusting laser power:
and (3) cooling rate regulation: adjusting laser power
For the same alloy melt, the cooling rate can be expressed according to temperature equation (1):
from equation (4), the alloy melt cooling rate gradually decreases as the applied laser power increases.
When the laser heating power and the radiation heat dissipation reach balance, the temperature change term at the left end of the equation (1) is zero, and then the following can be obtained:
according to equation (5), the effective laser power applied to the alloy melt surface is P E Can be kept at the set temperature T set 。
When the alloy melt is cooled to the temperature-controlled set temperature T set When the laser power is nearby, the PID temperature control system is used for adjusting the laser power:
wherein k is P 、k I 、k D The coefficients of the proportional term, the integral term and the differential term are respectively obtained. According to formula (6), the laser power is adjusted in real time, so that the alloy melt can be stably kept at a specified temperature.
And 7, when the alloy melt is kept at the set temperature, realizing solidification of the alloy melt. By triggering nucleation, the method has the advantage of realizing the active control of the solidification supercooling degree of the alloy melt.
Solidification example of a Si eutectic alloy melt at Nb-17.3 at.%:
1. establishing a temperature change equation of an alloy melt under the electrostatic suspension condition
The temperature change of the alloy melt under the electrostatic suspension condition is determined by the combined action of radiation heat dissipation and laser heating, and the equation is satisfied:
wherein m, A, C P T, ε are the mass (kg) and surface area (m) of the alloy melt, respectively 3 ) Specific heat (J.kg) -1 ·K -1 ) Temperature (K) and emissivity; sigma is Stefan-Boltzmann constant (5.06X10) -8 J·s -1 ·m -2 ·K -4 );T e Is the ambient temperature (298K); p (P) E Is the effective laser power (W) applied to the surface of the melt.
2. Alloy melt selection and parameter setting
Taking solidification condition control of Nb-17.3at.% Si eutectic alloy melt as an example, the density is 7320 kg.m -3 Specific heat of 380.4 J.kg -1 ·K -1 The heat radiation coefficient is 0.2065 and the eutectic temperatureA regulation mechanism for quantifying the cooling rate by the average cooling rate of the alloy melt between 200K super-heated above the eutectic temperature and 500K sub-cooled below the eutectic temperature (2389K-1689K).
3. Alloy melt cooling process under natural cooling condition
When no laser heating is performed, the static suspension alloy melt is cooled by radiating outwards in a natural radiation mode, and the right end term P in the equation (7) E =0, alloy melt temperature variation satisfies:
for a Nb-17.3at.% Si alloy melt of a specific diameter (d=6.0 mm), the cooling curve is shown in fig. 2, and the average cooling rate (2389K-1689K, hereinafter the same) is 58.7k·s -1 。
4. Cooling rate regulation mode one: varying alloy melt diameter
The temperature change equation (8) of the alloy melt under the natural cooling condition is rewritten into a form related to the melt diameter D:
according to equation (9), the cooling rate R of the alloy melt c Can be expressed as:
in the electrostatic suspension experiment, nb-17.3at.% Si eutectic alloy melt with the diameter of 1.0-6.0 mm is selected, and the average cooling rate can be regulated and controlled to 352.6-58.7Ks -1 . The quantitative relationship between the cooling curve and the average cooling rate and the alloy melt diameter is shown in FIG. 3.
5. And a second cooling rate regulation mode: adjusting laser power
For Nb-17.3at.% Si eutectic alloy melt with a diameter of 6mm, different laser power is applied to its surface, unlike the natural cooling process, where the heating laser is completely turned off. According to alloy melt temperature equation (7), its cooling rate can be expressed as:
the average cooling rate of Nb-17.3at.% Si eutectic alloy melt with the diameter of 6mm can be controlled to be 58.7-11.2 Ks when the effective laser power of 0-9.5W is applied -1 . The quantitative relationship between the cooling curve and the average cooling rate and the applied effective laser power is shown in fig. 4.
6. Alloy melt temperature control mode one: based on the heat balance equation
When the effective laser power absorbed by the surface of the alloy melt and the heat dissipation of outward radiation reach balance, the temperature of the alloy melt is kept unchanged. At this time, the left end temperature change term of equation (7) is zero, and can be rewritten as:
t in set For temperature control, the eutectic temperature (T) of the alloy and Nb-17.3at.% Si alloy E The difference =2189K) is the supercooling degree Δt of the melt. Determining the effective laser power P according to equation (12) E The relationship between the supercooling degree DeltaT of the alloy melt is set as shown in FIG. 5.
7. Alloy melt temperature control mode II: PID-based system
Initially, the laser is turned off. When the temperature of the Nb-17.3at.% Si eutectic alloy melt drops to T set And when the PID temperature control system is started, the laser power is adjusted:
k in P 、k I 、k D The coefficients of the proportional term, the integral term and the differential term are respectively obtained. When k is P 、k I 、k D Take the value 2 multiplied by 10 4 W·K -1 、2×10 2 W·K -1 ·s -1 、2×10 4 W·K -1 At s, the Nb-17.3at.% Si eutectic alloy melt is stably controlled within the supercooling range of 0 to 500K, as shown in FIG. 6.
8. When the Nb-17.3at.% Si eutectic alloy melt is kept at the set temperature, the alloy melt is solidified under different supercooling conditions by triggering nucleation, as shown in fig. 7, so that the active control of the solidification supercooling degree of the alloy melt is realized.
Claims (4)
1. A control method of the solidification condition of an electrostatic suspension alloy melt is characterized in that: controlling the cooling rate and supercooling degree of the alloy melt under the condition of electrostatic suspension:
step 1: in an ultrahigh vacuum electrostatic suspension experimental device, a spherical alloy sample is stably suspended in a strong electric field between an upper electrode and a lower electrode, and the alloy sample is in a melting overheat state by laser heating;
step 2, establishing a temperature change equation of the alloy melt:
wherein m, A, C P T and epsilon are the mass, surface area, specific heat, temperature and heat radiation coefficient of the alloy melt respectively; sigma is Stefan-Boltzmann constant; t (T) e Is the external environment temperature; p (P) E For an effective laser power applied to the melt surface;
left end of equationIndicating the temperature change of the alloy melt, radiating by radiation at the right end +.>And laser heating P E Determining the combined action;
step 3, regulating and controlling the cooling rate to enable the alloy melt to reduce the temperature according to the cooling rate: by varying the size of the alloy meltThe cooling rate is regulated and controlled, and the P is heated by the laser in the natural cooling process E =0, alloy melt temperature equation is:
cooling rate R c The method comprises the following steps:
the diameter D of the alloy melt is inversely proportional to the cooling rate, and the cooling rate is increased or decreased by reducing or increasing the diameter D of the alloy melt;
step 4, alloy melt temperature control: when the laser heating power and the radiation heat dissipation reach balance, the temperature change term of the heat balance equation in the step 2 is zero, and then:
by controlling the effective laser power applied to the alloy melt surface to be P according to the heat balance equation E Maintaining it at a set temperature T set ;
Step 5: when the alloy melt is kept at the set temperature, the solidification of the alloy melt is realized, and the active control of the solidification supercooling degree of the alloy melt is realized.
2. The method for controlling solidification conditions of an electrostatically suspended alloy melt as set forth in claim 1, wherein: the diameter of the spherical alloy sample is 1-6 mm.
3. The method for controlling solidification conditions of an electrostatically suspended alloy melt as set forth in claim 1, wherein: the cooling rate is regulated and controlled in the step 3, and the cooling rate is regulated and controlled by changing the laser power; according to the cooling rateThe laser power is inversely proportional to the alloy melt cooling rate, and by decreasing or increasing the laser power, the cooling rate is increased or decreased accordingly.
4. The method for controlling solidification conditions of an electrostatically suspended alloy melt as set forth in claim 1, wherein: the alloy melt temperature in the step 4 is controlled, when the alloy melt is cooled to the temperature control set temperature T set When the laser power is nearby, the PID temperature control system is used for adjusting the laser power:wherein k is P 、k I 、k D The laser power is regulated in real time according to the formula, so that the alloy melt is stably kept at the specified temperature. />
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