CN117026123B - A method and device for preparing metal materials by pulse ultrasonic coupling directional solidification technology - Google Patents
A method and device for preparing metal materials by pulse ultrasonic coupling directional solidification technology Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F3/00—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons
- C22F3/02—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons by solidifying a melt controlled by supersonic waves or electric or magnetic fields
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- Crystals, And After-Treatments Of Crystals (AREA)
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Abstract
本发明提供了一种脉冲超声耦合定向凝固技术制备金属材料的方法和装置，涉及金属制备技术领域。本发明提供的脉冲超声耦合定向凝固技术制备金属材料的方法，包括以下步骤：(1)将金属原料进行熔炼，得到金属熔体；(2)将所述金属熔体进行定向凝固，得到金属材料；在所述定向凝固过程中包括：向金属熔体施加脉冲超声。本发明通过在定向凝固过程中施加脉冲超声，调控定向组织的晶粒尺寸和生长取向，进一步优化其力学性能及其他功能特性。
The present invention provides a method and device for preparing metal materials by pulsed ultrasound coupled directional solidification technology, and relates to the technical field of metal preparation. The method for preparing metal materials by pulsed ultrasound coupled directional solidification technology provided by the present invention comprises the following steps: (1) smelting metal raw materials to obtain a metal melt; (2) directionally solidifying the metal melt to obtain a metal material; and the directional solidification process comprises: applying pulsed ultrasound to the metal melt. The present invention applies pulsed ultrasound during the directional solidification process to control the grain size and growth orientation of the directional structure, thereby further optimizing its mechanical properties and other functional characteristics.
Description
Technical Field
The invention relates to the technical field of metal preparation, in particular to a method and a device for preparing a metal material by using a pulse ultrasonic coupling directional solidification technology.
Background
Directional solidification is an advanced technology for preparing specific ordered tissue materials, and is an important means for researching solid-liquid phase change interface evolution rules. For metal materials, directional solidification is carried out by establishing a temperature gradient in a specific direction in solidified metal and non-solidified melt, so that the melt is solidified along the direction opposite to the heat flow, columnar crystals with specific orientation are obtained, and the aim of improving the longitudinal mechanical property of the material is fulfilled. The main control conditions of the traditional directional solidification technology include temperature gradient and drawing speed, so that the morphological characteristics and the ordering of a directional solidification structure can be regulated, however, the two parameters have limited regulation on the grain size of the columnar crystal in the directional growth process, and are often accompanied by transformation of the structure morphology (flat-cell-branch transformation), such as fine directional cell structure is difficult to obtain. In addition, the optimization effect of the traditional directional solidification on the aspects of columnar crystal growth orientation regulation, solute distribution and the like is limited.
In recent years, based on the combination of the conventional directional solidification technology and external field assistance, development of various novel directional solidification technologies has been paid attention to widely, such as directional solidification coupling electric fields, magnetic fields and the like. The ultrasonic field is used as a high-efficiency, high-energy and environment-friendly physical external field, and can cause a series of nonlinear effects including acoustic flow effect, cavitation effect, mechanical effect, thermal effect and the like in the melt, and has important influence on the processes of solution flow, diffusion of solute, solid phase particle diffusion, nucleation and growth of crystals, refinement of the crystals and the like, so that the effects of refining the crystals, ultrasonic degassing, inhibiting segregation and the like are realized.
However, coupling of ultrasound fields to directional solidification processes currently presents significant technical and technological difficulties. On one hand, the sound field at the front edge of the solid-liquid interface in the directional solidification process is subjected to complex and unknown changes due to complex solid-liquid phase load and acoustic impedance changes in the directional solidification process. On the other hand, as the stability of a liquid-solid interface needs to be maintained in the directional growth process, the interface temperature field may be unstable and the order of directional tissues is reduced due to the action of the ultra-strong ultrasound, and the action effect of the weak ultrasound on the directional growth process, particularly the refinement effect on the directional tissues, is limited.
Disclosure of Invention
The invention aims to provide a method and a device for preparing a metal material by a pulse ultrasonic coupling directional solidification technology, wherein the number of nucleation sites and growth characteristics of columnar crystals/dendrites are regulated and controlled by applying pulse ultrasonic vibration in the directional solidification process and acting on the front edge of a liquid-solid interface; the invention can detect the sound field characteristic at the front edge of the liquid-solid interface in the directional solidification process in real time and carry out feedback adjustment, thereby ensuring the high efficiency, stability and controllability of pulse ultrasonic treatment.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for preparing a metal material by a pulse ultrasonic coupling directional solidification technology, which comprises the following steps:
(1) Smelting a metal raw material to obtain a metal melt;
(2) Carrying out directional solidification on the metal melt to obtain a metal material; the directional solidification process comprises the following steps: pulsed ultrasound is applied to the metal melt.
Preferably, the directional solidification is performed under directional suction conditions; the speed of the directional drawing is 1-100 mu m/s.
Preferably, before pulse ultrasonic is applied to the metal melt, the metal melt is statically drawn for a distance h; the unit of h satisfying h 1<h<h2,h、h1 and h 2 is m; h 1 is the drawing distance when the columnar crystal just reaches stable directional growth; h 2 satisfies (k-1/4) c/2f 0<h2+L<(k+1/4)*c/2f0; wherein k is an integer, 0< k <10; c is the sound velocity of the ultrasonic amplitude transformer, and the unit is m/s; l is the total length of the ultrasonic amplitude transformer, and the unit is m; f 0 is the ultrasonic vibration treatment frequency, and the unit is kHz; f 0 satisfies 10kHz < f 0 <100kHz.
Preferably, the pulsed ultrasound consists of n pulse periods, wherein a single pulse period t=t 1+t2,t1 is the ultrasound action time, and t 2 is the ultrasound stop time; in the single pulse period t, the ultrasonic action time t 1 is greater than t 1',t1' and is the inoculation time of ultrasonic cavitation in the metal melt, and the time is the time required by the transient cavitation sound intensity to rise from 0 to the maximum value, and the unit is s; the ultrasonic stop time t 2 in a single pulse period is less than t 2',t2' which is the time required by the competition growth of columnar crystals and the stabilization of the columnar crystal directional tissue under the condition of the directional drawing speed, and the unit is s.
Preferably, the method for determining parameters of pulsed ultrasound comprises the following steps:
(1) When pulse ultrasound is started, detecting a sound spectrum signal at the front edge of a liquid-solid interface, extracting and analyzing to obtain transient cavitation sound intensity I, setting and inputting a cavitation threshold I 0, and adjusting A 0 to enable I=I 0,A0 to be the amplitude of the end face of an ultrasonic amplitude transformer;
(2) In the directional solidification process, the transient cavitation sound intensity I t at the front edge of the liquid-solid interface is obtained in real time, and the I t≥I0 is kept in the directional solidification process by regulating the A 0 through a computer.
The invention provides a device for the method in the technical scheme, which comprises a fixing system, a heating system, a heat insulation board, a cooling system, an ultrasonic system and an acoustic sensing system;
The heating system is arranged at the upper part of the heat insulation plate; the cooling system is arranged at the lower part of the heat insulation plate; the heating system, the heat insulation board and the cooling system are provided with central cavities which are communicated up and down;
a crucible is arranged in the central cavity;
the ultrasonic system comprises an ultrasonic amplitude transformer, an ultrasonic transducer and an ultrasonic power supply; the ultrasonic transducer is arranged at the tail part of the ultrasonic amplitude transformer; the ultrasonic transducer is connected with an ultrasonic power supply;
The fixation system includes a ram; the head of the pressure head is inserted into the top of the crucible; the head of the ultrasonic amplitude transformer is inserted into the bottom of the crucible through the central cavity; the crucible is clamped between the pressure head and the ultrasonic amplitude transformer;
the sound sensing system comprises a high-temperature acoustic sensor probe, a high-temperature piezoelectric conversion device and a computer; one end of the high-temperature acoustic sensor probe is arranged in the crucible; the other end of the high-temperature acoustic sensor probe is connected with a high-temperature piezoelectric conversion device; the high-temperature piezoelectric conversion device is connected with a computer;
the computer is connected with the ultrasonic power supply.
Preferably, the crucible is made of a high-temperature resistant material; the crucible is round in shape.
Preferably, the end surface of the ultrasonic amplitude transformer, which is in contact with the crucible, is provided with a first cylindrical boss; the first cylindrical boss is inserted into the bottom of the crucible; the outer diameter R 1 of the first cylindrical boss and the inner diameter R 0 of the crucible meet the requirements (R 1-R0)/R0>α1*(TL-T0+200),R0 and R 1 are in units of m, alpha 1 is the linear expansion coefficient of an ultrasonic amplitude transformer in units of m/K, T L is the liquidus temperature of metal in units of K, and T 0 is the temperature provided by a cooling system in units of K.
Preferably, the end face of the pressure head, which is contacted with the crucible, is provided with a second cylindrical boss; the second cylindrical boss is inserted into the top of the crucible; the outer diameter R 2 of the second cylindrical boss and the inner diameter R 0 of the crucible meet the requirements (R 2-R0)/R0>α2*(TL-T0+200),R0 and R 2 are in units of m, alpha 2 is the linear expansion coefficient of the pressure head and is in units of m/K, T L is the liquidus temperature of metal and is in units of K, and T 0 is the temperature provided by a cooling system and is in units of K.
Preferably, the fixation system further comprises a compression device; the pressing device is arranged at the tail part of the pressure head; the compressing device provides a pre-tightening force F for compressing the crucible, and the unit is N; f satisfies 10N < F <20N.
The invention provides a method for preparing a metal material by a pulse ultrasonic coupling directional solidification technology, which comprises the following steps: smelting a metal raw material to obtain a metal melt; (2) Carrying out directional solidification on the metal melt to obtain a metal material; the directional solidification process comprises the following steps: pulsed ultrasound is applied to the metal melt. The invention regulates and controls the grain size and growth orientation of directional tissue by applying pulse ultrasound in the directional solidification process, and further optimizes the mechanical property and other functional characteristics.
Preferably, the ultrasonic signal of the front edge of the liquid-solid interface in the directional solidification process can be detected and fed back and regulated in real time, so that the stability and controllability of pulse ultrasonic treatment are ensured.
Specifically, in the process of directional solidification dynamic drawing, pulse ultrasonic vibration is applied to the crucible to act on the front edge of a liquid-solid interface of the metal melt, so that the orientation and the grain size of columnar crystal directional growth are regulated and controlled. By controlling the conditions of the frequency, amplitude, pulse duty ratio and the like of the pulse ultrasound, the fine crystal effect of the ultrasound is fully utilized on the premise of not damaging the directional growth stability, and the preparation of the superfine directional tissue is realized under the conditions of limited temperature gradient and drawing rate. Aiming at the action effect of the ultrasound at different stages of the directional solidification process, corresponding ultrasound signals at different positions are detected in real time and are subjected to feedback adjustment, so that the high efficiency, stability and controllability of the ultrasound treatment are ensured. Based on the method, the mechanical property of the metal material is improved through fine grain strengthening, and the comprehensive regulation and control of the application performance of the metal material is realized through the control and control function characteristics of directional growth orientation.
The method provided by the invention has the advantages of green, environment-friendly, high-efficiency, energy-saving and the like, the size of columnar crystals in the prepared metal material is obviously thinned, meanwhile, the better directional growth characteristic is reserved, and the mechanical property of the metal material is obviously improved.
Drawings
FIG. 1 is a schematic diagram of an apparatus for preparing a metallic material by a pulsed ultrasonic coupled directional solidification technique; in fig. 1, 1 is a cylinder, 2 is a high Wen Yatou, 3 is a high-frequency induction coil, 4 is a heat insulation plate, 5 is a liquid cooling tank, 6 is a high-temperature acoustic sensor probe, 7 is a high-temperature piezoelectric conversion device, 8 is a computer, 9 is an ultrasonic power supply, 10 is an ultrasonic transducer, and 11 is an ultrasonic amplitude transformer;
FIG. 2 is a flow chart of a method of preparing a metallic material by pulsed ultrasonic coupling directional solidification technique in an embodiment;
FIG. 3 is a real-time monitoring of a pulse sound signal during a pull process;
FIG. 4 is a microstructure comparison chart of Cu-14wt.% Al-4.5wt.% Ni alloy in example 1 and comparative examples 1-2;
FIG. 5 is a graph comparing tensile properties at 20℃of Cu-14wt.% Al-4.5wt.% Ni alloys in example 1 and comparative examples 1-2;
FIG. 6 is a graph showing a 200 ℃ tensile property comparison of Cu-14wt.% Al-4.5wt.% Ni alloys in example 1 and comparative examples 1-2.
Detailed Description
The invention provides a method for preparing a metal material by a pulse ultrasonic coupling directional solidification technology, which comprises the following steps:
(1) Smelting a metal raw material to obtain a metal melt;
(2) Carrying out directional solidification on the metal melt to obtain a metal material; the directional solidification process comprises the following steps: pulsed ultrasound is applied to the metal melt.
The invention smelts the metal raw material to obtain the metal melt. In the present invention, the metal raw material preferably includes a pure metal or an alloy.
In the present invention, the smelting of the metal raw material preferably includes: firstly, carrying out primary smelting on a metal raw material to obtain a master metal ingot; cutting the mother metal ingot to obtain a metal rod; and heating and preserving the heat of the metal rod. In the present invention, the smelting is preferably performed in vacuum or in a protective atmosphere. In the present invention, the diameter of the metal rod is preferably smaller than the inner diameter of the crucible. In the invention, the temperature of heating and heat preservation is preferably 100-200K higher than the liquidus line of the metal; the heating and heat-preserving time is preferably 20-40 min, more preferably 30min. In the present invention, the heating and heat preservation are preferably performed under a standing condition.
After the metal melt is obtained, the metal melt is directionally solidified to obtain the metal material. The invention comprises the following steps in the directional solidification process: pulsed ultrasound is applied to the metal melt. In the present invention, the directional solidification is preferably performed in a protective atmosphere. In the present invention, the method of providing the protective atmosphere preferably includes: vacuum was pulled to P 1 and protective gas was introduced to pressure P 2. In the present invention, the pressure of P 1 is preferably less than 0.01Pa, and the pressure of P 2 is preferably 100 to 5000Pa. The invention can prevent metal oxidation in the smelting process and can also prevent gas expansion by heating beyond one atmosphere by adopting the conditions. In the present invention, the protective gas preferably includes argon; the flow rate of the protective gas is preferably 2-3L/min.
In the present invention, the directional solidification is preferably performed under a directional pumping condition; the speed of the directional drawing is preferably 1 to 100 μm/s.
In the invention, before pulse ultrasonic is applied to the metal melt, the metal melt is preferably drawn statically for a distance h; the units of h preferably satisfying h 1<h<h2,h、h1 and h 2 are m; h 1 is the drawing distance when the columnar crystal just reaches stable directional growth; h 2 satisfies (k-1/4) c/2f 0<h2+L<(k+1/4)*c/2f0; wherein k is an integer, 0< k <10; c is the sound velocity of the ultrasonic amplitude transformer, and the unit is m/s; l is the total length of the ultrasonic amplitude transformer, and the unit is m; f 0 is the ultrasonic vibration treatment frequency, and the unit is kHz; f 0 satisfies 10kHz < f 0 <100kHz. In the invention, h 1 can be obtained according to directional experiment statistics; and h 2 is a minimum value for ensuring that the end face of the solid-liquid interface is positioned near the integral resonance point of the vibration system.
In the present invention, the pulsed ultrasound is preferably composed of n pulse periods, wherein a single pulse period t=t 1+t2,;t1 is the ultrasound action time and t 2 is the ultrasound stop time. In the invention, in the single pulse period t, the ultrasonic action time t 1 is preferably greater than t 1',t1' and is the inoculation time of ultrasonic cavitation in the metal melt, wherein the time is the time required by the transient cavitation sound intensity to rise from 0 to the maximum value, and the unit is s; the ultrasonic stop time t 2 in a single pulse period is preferably less than t 2',t2' which is the time required for the competing growth of columnar crystals and the stabilization of the columnar crystal orientation tissue under the condition of the orientation drawing speed, and the unit is s. In the invention, t 1' is obtained by detecting sound field information at the front edge of a liquid-solid interface through an acoustic sensing system; the t 2' can be obtained according to directional experimental statistics.
In the present invention, the method for determining parameters of pulsed ultrasound preferably includes:
(1) When pulse ultrasound is started, detecting a sound spectrum signal at the front edge of a liquid-solid interface, extracting and analyzing to obtain transient cavitation sound intensity I, setting and inputting a cavitation threshold I 0, and adjusting A 0 to enable I=I 0,A0 to be the amplitude of the end face of an ultrasonic amplitude transformer;
(2) In the directional solidification process, the transient cavitation sound intensity I t at the front edge of the liquid-solid interface is obtained in real time, and the I t≥I0 is kept in the directional solidification process by regulating the A 0 through a computer.
In the present invention, the units of I, I 0 and I t are W/m 2; the unit of A 0 is μm.
The invention provides a device for the method in the technical proposal, which is shown in figure 1 and comprises a fixing system, a heating system, a heat insulation board, a cooling system, an ultrasonic system and an acoustic sensing system;
The heating system is arranged at the upper part of the heat insulation plate; the cooling system is arranged at the lower part of the heat insulation plate; the heating system, the heat insulation board and the cooling system are provided with central cavities which are communicated up and down;
a crucible is arranged in the central cavity;
the ultrasonic system comprises an ultrasonic amplitude transformer, an ultrasonic transducer and an ultrasonic power supply; the ultrasonic transducer is arranged at the tail part of the ultrasonic amplitude transformer; the ultrasonic transducer is connected with an ultrasonic power supply;
The fixation system includes a ram; the head of the pressure head is inserted into the top of the crucible; the head of the ultrasonic amplitude transformer is inserted into the bottom of the crucible through the central cavity; the crucible is clamped between the pressure head and the ultrasonic amplitude transformer;
the sound sensing system comprises a high-temperature acoustic sensor probe, a high-temperature piezoelectric conversion device and a computer; one end of the high-temperature acoustic sensor probe is arranged in the crucible; the other end of the high-temperature acoustic sensor probe is connected with a high-temperature piezoelectric conversion device; the high-temperature piezoelectric conversion device is connected with a computer;
the computer is connected with the ultrasonic power supply.
As an embodiment of the invention, the fixation system further comprises a compression device; the pressing device is arranged at the tail part of the pressure head; the compressing device provides a pre-tightening force F for compressing the crucible, and the unit is N; f satisfies 10N < F <20N. In the present invention, the pressing means preferably includes a cylinder or a spring.
As one embodiment of the invention, the heating system comprises a graphite heating sleeve, a mullite heat preservation sleeve, a quartz protection cover and a high-frequency induction coil which are sequentially arranged on the periphery of the crucible;
as one embodiment of the invention, the heat insulation plate is made of quartz or boron nitride; the thickness of the insulation panel is preferably greater than 5mm.
As one embodiment of the present invention, the cooling system includes a liquid cooling tank and a liquid metal placed in the liquid cooling tank; the liquid metal preferably comprises Ga, in and Sn; the mass ratio of Ga, in and Sn In the liquid metal is preferably 68.5:21.5:10.
As an embodiment of the present invention, the crucible is made of a high temperature resistant material, and is preferably high-purity corundum or graphite; the crucible is circular in shape; the wall thickness of the crucible is preferably less than 2mm. In the invention, an ultrasonic amplitude transformer is arranged at the bottom of the crucible, and a pressure head is arranged at the top of the crucible.
As one embodiment of the invention, the Young's modulus of the material of the ultrasonic horn is greater than 50GPa at the extreme withstand temperature (T L +200K). In the invention, T L is the liquidus temperature of the prepared metal material, and the unit is K.
As one embodiment of the invention, the ultrasonic amplitude transformer is cylindrical in shape, and a first cylindrical boss is arranged on the end surface of the ultrasonic amplitude transformer, which is in contact with the crucible; the first cylindrical boss is inserted into the bottom of the crucible; the outer diameter R 1 of the first cylindrical boss and the inner diameter R 0 of the crucible meet the requirements (R 1-R0)/R0>α1*(TL-T0+200),R0 and R 1 are in units of m, alpha 1 is the linear expansion coefficient of an ultrasonic amplitude transformer in units of m/K, T L is the liquidus temperature of metal in units of K, and T 0 is the temperature provided by a cooling system in units of K.
As an embodiment of the invention, the ram is high Wen Yatou; the Young modulus of the material of the high-temperature pressure head is higher than 50GPa when T L +200K is satisfied.
As one embodiment of the invention, the pressure head is cylindrical in shape, and a through groove is formed along the central axis direction of the cylindrical pressure head and is used for placing a high-temperature acoustic sensor probe; the end face of the pressure head, which is in contact with the crucible, is provided with a second cylindrical boss; the second cylindrical boss is inserted into the top of the crucible; the outer diameter R 2 of the second cylindrical boss and the inner diameter R 0 of the crucible meet the requirements (R 2-R0)/R0>α2*(TL-T0+200),R0 and R 2 are in units of m, alpha 2 is the linear expansion coefficient of the pressure head and is in units of m/K, T L is the liquidus temperature of metal and is in units of K, and T 0 is the temperature provided by a cooling system and is in units of K.
As an embodiment of the present invention, the material of the high-temperature acoustic sensor probe is preferably a metal with a melting point of 2000 ℃ or higher and stable physicochemical properties, and is particularly preferably tungsten, molybdenum or niobium; the diameter of the high temperature acoustic sensor probe is preferably less than 1.5mm.
As an embodiment of the present invention, as shown in fig. 1, a method for preparing a metal material by a pulsed ultrasonic coupling directional solidification technology includes: placing the crucible in a heating system, and placing a metal raw material in the crucible for smelting to obtain a metal melt; the fixing system, the crucible and the ultrasonic system are kept motionless, the heating system, the heat insulation plate and the cooling system are synchronously moved upwards, so that the metal melt in the crucible is subjected to directional drawing in the cooling system, pulse ultrasonic is simultaneously started after a certain distance is drawn, sound field information at the front edge of a liquid-solid interface is detected through the acoustic sensing system, and real-time feedback adjustment is performed by combining the detection result; stopping moving after the metal melt is completely solidified, and taking out the sample after cooling to obtain the metal material. In a specific embodiment of the present invention, detecting sound field information at a liquid-solid interface front by an acoustic sensing system includes: and inserting the high-temperature acoustic sensor probe into the crucible to enable the high-temperature acoustic sensor probe to be positioned at the front edge of the liquid-solid interface, and obtaining sound field information at the front edge of the liquid-solid interface. In a specific embodiment of the present invention, the real-time feedback adjustment is as shown in fig. 3, and the process is as follows: when pulse ultrasound is started, detecting a sound spectrum signal at the front edge of a liquid-solid interface through an acoustic sensing system, extracting and analyzing to obtain transient cavitation sound intensity I, setting and inputting a cavitation threshold I 0, and adjusting A 0 to enable I=I 0,A0 to be the amplitude of the end face of an ultrasonic amplitude transformer; in the directional solidification process, the transient cavitation sound intensity I t at the front edge of the liquid-solid interface is obtained in real time, and the I t≥I0 is kept in the directional solidification process by regulating the A 0 through a computer.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment is a method for preparing Cu-14wt.% Al-4.5wt.% Ni alloy by using a pulse ultrasonic coupling directional solidification technology, wherein a flow chart is shown in fig. 2, a schematic diagram of an adopted device is shown in fig. 1, and the steps are as follows:
Loading 280g of high-purity Al blocks and 1630g of high-purity Cu blocks into a graphite crucible with the internal dimension phi of 100mm multiplied by 100mm, introducing argon with the air flow of 2.5L/min for induction heating smelting, and preserving heat for 5min after the smelting temperature reaches 1100 ℃; then adding 90g of high-purity Ni blocks, increasing induction current, raising the smelting temperature to 1300 ℃, and preserving the heat for 1min; properly adjusting heating current, continuously preserving heat and refining for 2min at 1100 ℃ to obtain a master alloy ingot, and cutting a raw material rod with the diameter of 9.5mm and the length of 100mm from the master alloy ingot;
A corundum (Al 2O3, purity is 99 wt%) crucible with an inner diameter of 10mm, a wall thickness of 2mm and a length of 140mm is placed on a first cylindrical boss at the upper end of an ultrasonic amplitude transformer, the first cylindrical boss is inserted into the crucible from the lower part, and the ultrasonic amplitude transformer is made of TC4 titanium alloy. And then placing the two raw material rods into a crucible from the upper part, and installing a heating system (a graphite heating sleeve, a mullite heat preservation sleeve, a quartz protection cover and a high-frequency induction coil which are sequentially arranged on the periphery of the crucible) around the crucible. The high-temperature pressing head is arranged right above the crucible, a second cylindrical boss is arranged at the lower end of the high-temperature pressing head, the second cylindrical boss is inserted into the crucible from the upper part, and the high-temperature pressing head is made of niobium. The pretightening force F is regulated by an air cylinder arranged on the upper end surface of the high-temperature pressure head, so that it satisfies 10N < F <20N.
And placing the high-temperature acoustic sensor probe into the crucible through a penetrating groove with the height Wen Yatou, wherein the high-temperature acoustic sensor probe is made of molybdenum. The testing end face of the high-temperature acoustic sensor probe is positioned on the central axis of the crucible, and the output end face of the high-temperature acoustic sensor probe is connected with the high-temperature piezoelectric conversion device. The high-temperature piezoelectric conversion device is fixed on the displacement table, the displacement table is fixed on the heat insulation plate, the displacement table can move along with the heat insulation plate in the drawing process, and meanwhile, the height of the testing end face of the high-temperature acoustic sensor probe on the central axis of the crucible can be adjusted. A cooling system is arranged below the heat insulation plate and consists of a liquid cooling tank and liquid metal placed in the liquid cooling tank; the liquid cooling tank is filled with liquid metal, and the liquid metal comprises the components of Ga: in: sn=68.5%: 21.5%:10% (wt.).
The heating system, the heat insulation plate and the cooling system are provided with a central cavity which is communicated up and down, and the crucible is arranged in the central cavity; the heating system, the heat insulating plate and the cooling system are fixed on a positioning platform together.
Argon is introduced into the quartz protective cover for atmosphere protection, and the flow rate of the argon is 2L/min. And starting high-frequency induction, heating by a high-frequency induction coil, and standing for 30min after the alloy melt in the crucible reaches 1200 ℃. After the heat preservation is finished, a displacement table below the high-temperature piezoelectric conversion device is moved, so that the testing end face of the high-temperature acoustic sensor probe moves downwards until touching a solid-liquid interface, then moves upwards by 15mm and locks the displacement table. And controlling a motor to enable the positioning platform to move upwards at a constant drawing speed of 100 mu m/s so as to carry out static directional drawing. Pulse ultrasound is started after static pulling for 3cm, the vibration treatment frequency f 0 =20 kHz of the ultrasound, and the initial amplitude a 0 =8.7 μm; the pulse period is 2s, wherein the time proportion of the ultrasonic is 50 percent, namely the ultrasonic stops for 1s after working for 1s; the total time of the entire pulsed ultrasound was 10min. At the same time, the acoustic sensing system is turned on to detect the acoustic signal generated by the pulsed ultrasound, as shown in fig. 3. And extracting and analyzing the processed signals to obtain transient cavitation sound intensity I t, inputting a set cavitation threshold I 0, and regulating ultrasonic amplitude through a computer to enable I t≥I0. And after the drawing is finished, turning off the power supply, and taking out after the sample is cooled to obtain the Cu-14wt.% Al-4.5wt.% Ni alloy.
Comparative example 1
The preparation process was essentially the same as in example 1, except that pulsed ultrasound was not performed during the drawing.
Comparative example 2
The preparation method is basically the same as that of the example 1, except that the pulse ultrasound is adjusted to be uninterrupted ultrasound, and the pulse period is 2s, wherein the time ratio of the ultrasound is 50%, namely, the ultrasound is stopped for 1s after 1s of operation; the total time of the entire pulsed ultrasound was 10min "adjusted to" continue to apply ultrasound for 10min ".
Test case
As shown in fig. 4, the directional structure of comparative example 1 (fig. 4 (a)) and example 1 (fig. 4 (b)) was compared, and it was found that the columnar crystal grain size was significantly refined while retaining the directional growth characteristics thereof under the pulsed ultrasonic action, whereas in comparative example 2 (fig. 4 (c)), the directional characteristics thereof were substantially destroyed although the columnar crystal grain size was significantly refined.
Tensile properties of Cu-14wt.% Al-4.5wt.% Ni alloys prepared in example 1 and comparative examples 1-2 are shown in FIGS. 5-6 and Table 1. The superelastic strain rate is the strain rate that continues to occur after the end of the yield phase of the tensile curve, i.e., the strain rate value from the second abrupt change in stress/strain slope to the fracture of the specimen.
TABLE 1 tensile Properties of the alloys prepared in example 1 and comparative examples 1-2
Comparing the tensile properties of fig. 5-6 and table 1, it was found that the yield strength of the alloy of example 1 at room temperature and 200 c was improved by a factor of 1.6 and 1.5, respectively, compared to comparative example 1, while maintaining the original superelasticity (i.e., the stress/strain slope that continued after the end of the yield phase was close to the deformation at the elastic deformation phase), whereas the yield strength of the alloy of comparative example 2 was improved but the superelasticity was substantially lost.
For the shape recovery characteristics of the alloys, the shape recovery test method in table 1 is: under the condition of 200 ℃ (higher than the martensite transformation temperature of the alloy), the strain recovery is carried out after the strain rate of the sample reaches 3.2% through high-temperature stretching, and the strain recovery condition is detected. The shape recovery of the alloy prepared in example 1 was higher due to better retention of the directional growth characteristics, consistent with comparative example 1, while the recovery was reduced to 73.7% due to the failure of the directional characteristics in comparative example 2.
Based on the comparison, the method for preparing the metal material by the pulse ultrasonic coupling directional solidification technology provided by the invention applies pulse ultrasonic vibration to the crucible in the process of directional solidification dynamic drawing, acts on the front edge of a melt liquid-solid interface, and regulates and controls the orientation and grain size of columnar crystal directional growth. Aiming at the effect of the ultrasound at different stages of the directional solidification process, corresponding ultrasound signals at different positions are detected in real time and are subjected to feedback regulation, so that the high efficiency, stability and controllability of the ultrasound treatment are ensured, the mechanical properties of the metal material are improved through fine crystal strengthening based on the high efficiency, stability and controllability of the ultrasound treatment, and the functional characteristics are regulated and controlled through the control of the directional growth orientation.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (9)
1. A method for preparing a metal material by a pulse ultrasonic coupling directional solidification technology comprises the following steps:
(1) Smelting a metal raw material to obtain a metal melt;
(2) Carrying out directional solidification on the metal melt to obtain a metal material; the directional solidification process comprises the following steps: applying pulsed ultrasound to the metal melt;
The parameter determination method of the pulse ultrasound comprises the following steps:
(1) When pulse ultrasound is started, detecting a sound spectrum signal at the front edge of a liquid-solid interface, extracting and analyzing to obtain transient cavitation sound intensity I, setting and inputting a cavitation threshold I 0, and adjusting A 0 to enable I=I 0,A0 to be the amplitude of the end face of an ultrasonic amplitude transformer;
(2) In the directional solidification process, the transient cavitation sound intensity I t at the front edge of the liquid-solid interface is obtained in real time, and the I t≥I0 is kept in the directional solidification process by regulating the A 0 through a computer.
2. The method of claim 1, wherein the directional solidification is performed under directional suction conditions; the speed of the directional drawing is 1-100 mu m/s.
3. The method according to claim 2, characterized in that the metal melt is drawn statically for a distance h before pulsed ultrasound is applied to the metal melt; the unit of h satisfying h 1<h<h2,h、h1 and h 2 is m; h 1 is the drawing distance when the columnar crystal just reaches stable directional growth; h 2 satisfies (k-1/4) c/2f 0<h2+L<(k+1/4)*c/2f0; wherein k is an integer, 0< k <10; c is the sound velocity of the ultrasonic amplitude transformer, and the unit is m/s; l is the total length of the ultrasonic amplitude transformer, and the unit is m; f 0 is the ultrasonic vibration treatment frequency, and the unit is kHz; f 0 satisfies 10kHz < f 0 <100kHz.
4. The method of claim 2, wherein the pulsed ultrasound consists of n pulse periods, wherein a single pulse period t = t 1+t2,t1 is an ultrasound on time, and t 2 is an ultrasound off time; in the single pulse period t, the ultrasonic action time t 1 is greater than t 1',t1' and is the inoculation time of ultrasonic cavitation in the metal melt, and the time is the time required by the transient cavitation sound intensity to rise from 0 to the maximum value, and the unit is s; the ultrasonic stop time t 2 in a single pulse period is less than t 2',t2' which is the time required by the competition growth of columnar crystals and the stabilization of the columnar crystal directional tissue under the condition of the directional drawing speed, and the unit is s.
5. The method according to any one of claims 1 to 4, wherein the means for the method comprises a fixing system, a heating system, a heat shield, a cooling system, an ultrasound system and an acoustic sensing system;
The heating system is arranged at the upper part of the heat insulation plate; the cooling system is arranged at the lower part of the heat insulation plate; the heating system, the heat insulation board and the cooling system are provided with central cavities which are communicated up and down;
a crucible is arranged in the central cavity;
the ultrasonic system comprises an ultrasonic amplitude transformer, an ultrasonic transducer and an ultrasonic power supply; the ultrasonic transducer is arranged at the tail part of the ultrasonic amplitude transformer; the ultrasonic transducer is connected with an ultrasonic power supply;
The fixation system includes a ram; the head of the pressure head is inserted into the top of the crucible; the head of the ultrasonic amplitude transformer is inserted into the bottom of the crucible through the central cavity; the crucible is clamped between the pressure head and the ultrasonic amplitude transformer;
the sound sensing system comprises a high-temperature acoustic sensor probe, a high-temperature piezoelectric conversion device and a computer; one end of the high-temperature acoustic sensor probe is arranged in the crucible; the other end of the high-temperature acoustic sensor probe is connected with a high-temperature piezoelectric conversion device; the high-temperature piezoelectric conversion device is connected with a computer;
the computer is connected with the ultrasonic power supply.
6. The method of claim 5, wherein the crucible is a high temperature resistant material; the crucible is round in shape.
7. The method of claim 5 wherein the end face of the ultrasonic horn in contact with the crucible is provided with a first cylindrical boss; the first cylindrical boss is inserted into the bottom of the crucible; the outer diameter R 1 of the first cylindrical boss and the inner diameter R 0 of the crucible meet the requirements (R 1-R0)/R0>α1*(TL-T0+200),R0 and R 1 are in units of m, alpha 1 is the linear expansion coefficient of an ultrasonic amplitude transformer in units of m/K, T L is the liquidus temperature of metal in units of K, and T 0 is the temperature provided by a cooling system in units of K.
8. The method of claim 5, wherein the end face of the ram in contact with the crucible is provided with a second cylindrical boss; the second cylindrical boss is inserted into the top of the crucible; the outer diameter R 2 of the second cylindrical boss and the inner diameter R 0 of the crucible meet the requirements (R 2-R0)/R0>α2*(TL-T0+200),R0 and R 2 are in units of m, alpha 2 is the linear expansion coefficient of the pressure head and is in units of m/K, T L is the liquidus temperature of metal and is in units of K, and T 0 is the temperature provided by a cooling system and is in units of K.
9. The method of claim 5, wherein the fixation system further comprises a compression device; the pressing device is arranged at the tail part of the pressure head; the compressing device provides a pre-tightening force F for compressing the crucible, and the unit is N; f satisfies 10N < F <20N.
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