A kind of oxygen inhalation under pressure method for annealing of REBCO superconductor
Technical field
The present invention relates to superconductor preparation field, the pressurization that is specifically related to a kind of REBCO superconductor is inhaledOxygen method for annealing.
Background technology
Superconductor is under certain cryogenic conditions, to present that resistance equals zero and certain diamagnetic materialMaterial, can be widely used in making the fields such as superconductive current limiter, superconducting magnet and power cable. REBCO (REFor rare earth elements such as Y, Gd, Sm, Nd, Dy) as a kind of high temperature superconducting materia, because having height, it facesBoundary's temperature, high critical current and in magnetic field better superconductivity, become gradually in recent years superconductionStudy hotspot in material.
REBCO(REBa2Cu3O7-x, wherein x is 0≤x≤0.6) and superconductor belongs to complicated perovskite structure,Its oxygen content is not 7 under perfect condition conventionally, when oxygen content x gradually changes to 0.6 time by 0, and superconductionThe structure of material turns to Tetragonal by orthogonal phase transformation, and the superconductivity of material fades away. But oxygen contentNot more high better, appropriate oxygen defect can be introduced defect in material, plays the object of pinning magnetic flux.Therefore, in the time of preparation high-performance REBCO superconductor, the oxygen content of easier its inside configuration of control of energySeem particularly important.
Research shows, the oxygen content in REBCO material and annealing process and ambient oxygen partial pressure are closely related. ExistingIn some REBCO superconductor annealing processes, its inner oxygen content is conventionally by optimizing annealing temperature and annealingTime is controlled. Now conventional annealing process often exists that oxygen uptake is insufficient and annealing time is longProblem. On the one hand, oxygen uptake is insufficient can affect REBCO superconductor critical electric current value; Annealing on the other handTime, long meeting affect production efficiency.
Therefore, how REBCO superconductor preparation field, realize and enhancing productivity and superconduction material nowThe sufficient technique of material oxygen uptake is letter problem to be solved in whole superconductor field.
Summary of the invention
The object of the invention is to overcome the above problem that prior art exists, a kind of REBCO superconduction is providedThe oxygen inhalation under pressure method for annealing of material, the oxygen inhalation under pressure method for annealing of above-mentioned REBCO superconductor is in superconductionIn anneal of material process, introduce a new oxygen pressure technological parameter, increased and increase oxygen pressure techniqueControl, make superconductor oxygen uptake in oxygen uptake annealing process more abundant.
For realizing above-mentioned technical purpose, reach above-mentioned technique effect, the present invention is real by the following technical programsExisting:
An oxygen inhalation under pressure method for annealing for REBCO superconductor, is characterized in that, comprises the following steps:
S100: preparation REBCO superconductor, described REBCO superconductor comprise REBCO superconducting layer andBe arranged on the Ag stabilized zone on described REBCO superconducting layer;
S200: described REBCO superconductor is put in annealing furnace;
S300: will vacuumize in described annealing furnace;
S400: be filled with oxygen in described annealing furnace, described annealing furnace is provided with pressure regulator valve, by describedPressure regulator valve regulates the oxygen pressure in described annealing furnace, and oxygen pressure in described annealing furnace is minimum is 1atm;
S500: described annealing furnace heats up, and is warming up to annealing temperature, and described annealing temperature is 450 DEG C-550 DEG C,Control heating rate and be no more than 6 DEG C/min;
In S600:S500, reach after annealing temperature, keep annealing temperature constant temperature, make described REBCO superconductionThe abundant oxygen uptake of material;
S700: described annealing furnace is cooled to room temperature, controls rate of temperature fall and is no more than 1 DEG C/min;
S800: take out the described REBCO superconductor after oxygen inhalation under pressure annealing, to described REBCO superconductionMaterial carries out critical current test.
Preferably, in described S400, regulate oxygen pressure to the above 0-0.05MPa of 1atm by pressure regulator valve.
Preferably, the annealing temperature in described S500 is 500 DEG C, and heating rate is 3-6 DEG C/min.
Preferably, in described S600, constant temperature time is 4-6h.
Preferably, in described S700, rate of temperature fall is 0.5-1 DEG C/min.
Preferably, in described S800, detect the critical electric current value of described REBCO superconductor, as described S400When middle oxygen pressure is 0.015MPa, the critical electric current value of described REBCO superconductor is the highest, described inThe oxygen content of REBCO superconductor is in good state.
The invention has the beneficial effects as follows:
The oxygen inhalation under pressure method for annealing of one, REBCO superconductor disclosed by the invention moves back at superconductorIn fire process, introduce a new oxygen pressure technological parameter, increased the control that increases oxygen pressure technique,Make superconductor oxygen uptake in oxygen uptake annealing process more abundant.
Two, the oxygen inhalation under pressure method for annealing technique of REBCO superconductor of the present invention is simple, by rightThe control of oxygen pressure, can increase the diffusion rate of oxygen in superconductor, and superconductor is being moved backIn fire process, oxygen uptake is more abundant, thereby increases the critical electric current value of superconductor; And can be high in guaranteeIn the situation of critical electric current value, reduce annealing time, improved production efficiency.
Three, the oxygen inhalation under pressure method for annealing technological parameter controllability of REBCO superconductor of the present invention is good,For example, annealing temperature, annealing time, heating rate, rate of temperature fall are easy to adjust, make this technique energyEnough extensive uses.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand skill of the present inventionArt means, and can being implemented according to the content of description, below with preferred embodiment of the present invention and joinClosing accompanying drawing is described in detail as follows. The specific embodiment of the present invention is given in detail by following examples and accompanying drawing thereofGo out.
Brief description of the drawings
In order to be illustrated more clearly in the technical scheme in embodiment of the present invention technology, below will be to embodiment skillIn art description, the accompanying drawing of required use is briefly described, apparently, and the accompanying drawing in the following describesBe only some embodiments of the present invention, for those of ordinary skill in the art, do not paying creationUnder the prerequisite of property work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is that REBCO superconductor critical current of the present invention is with different oxygen pressure situation of change figure.
Wherein, abscissa is oxygen pressure, and ordinate is critical electric current value.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried outDescribe clearly and completely, obviously, described embodiment is only the present invention's part embodiment, andNot whole embodiment. Based on the embodiment in the present invention, those of ordinary skill in the art are not doingGo out the every other embodiment obtaining under creative work prerequisite, all belong to the scope of protection of the invention.
Embodiment 1
The oxygen inhalation under pressure method for annealing that discloses a kind of REBCO superconductor in embodiment 1, mainly comprisesFollowing steps:
S100: preparation REBCO superconductor, above-mentioned REBCO superconductor comprise REBCO superconducting layer andBe arranged on the Ag stabilized zone on above-mentioned REBCO superconducting layer.
S200: above-mentioned REBCO superconductor is put in annealing furnace.
S300: will in above-mentioned annealing furnace, vacuumize, while ensureing the annealing of above-mentioned REBCO superconductor at oxygenUnder atmosphere, carry out.
S400: be filled with oxygen in above-mentioned annealing furnace, above-mentioned annealing furnace is provided with pressure regulator valve, by above-mentionedPressure regulator valve regulates the oxygen pressure in above-mentioned annealing furnace, and the oxygen pressure in above-mentioned annealing furnace is 1atm;
S500: above-mentioned annealing furnace heats up, and is warming up to annealing temperature, and above-mentioned annealing temperature is 450 DEG C, controlsApproximately 3 DEG C/min of heating rate, the 100min that approximately heats up is to above-mentioned annealing temperature.
In S600:S500, reach after 450 DEG C of annealing temperatures, keep annealing temperature constant temperature, constant temperature 4h, makesState the abundant oxygen uptake of REBCO superconductor;
S700: above-mentioned annealing furnace is cooled to room temperature, is cooled to room temperature by 450 DEG C, controls rate of temperature fall to be0.5℃/min。
S800: take out the above-mentioned REBCO superconductor after oxygen inhalation under pressure annealing, to above-mentioned REBCO superconductionMaterial carries out critical current test.
Embodiment 2
The oxygen inhalation under pressure method for annealing that discloses a kind of REBCO superconductor in embodiment 2, mainly comprisesFollowing steps:
S100: preparation REBCO superconductor, above-mentioned REBCO superconductor comprise REBCO superconducting layer andBe arranged on the Ag stabilized zone on above-mentioned REBCO superconducting layer.
S200: above-mentioned REBCO superconductor is put in annealing furnace.
S300: will in above-mentioned annealing furnace, vacuumize, while ensureing the annealing of above-mentioned REBCO superconductor at oxygenUnder atmosphere, carry out.
S400: be filled with oxygen in above-mentioned annealing furnace, above-mentioned annealing furnace is provided with pressure regulator valve, by above-mentionedPressure regulator valve regulates the oxygen pressure in above-mentioned annealing furnace, the oxygen pressure in above-mentioned annealing furnace be 1atm withUpper 0.010MPa;
S500: above-mentioned annealing furnace heats up, and is warming up to annealing temperature, and above-mentioned annealing temperature is 500 DEG C, controlsApproximately 5 DEG C/min of heating rate, the 100min that approximately heats up is to above-mentioned annealing temperature.
In S600:S500, reach after 500 DEG C of annealing temperatures, keep annealing temperature constant temperature, constant temperature 5h, makesState the abundant oxygen uptake of REBCO superconductor;
S700: above-mentioned annealing furnace is cooled to room temperature, is cooled to room temperature by 500 DEG C, controls rate of temperature fall0.5℃/min。
S800: take out the above-mentioned REBCO superconductor after oxygen inhalation under pressure annealing, to above-mentioned REBCO superconductionMaterial carries out critical current test.
Embodiment 3
The oxygen inhalation under pressure method for annealing that discloses a kind of REBCO superconductor in embodiment 3, mainly comprisesFollowing steps:
S100: preparation REBCO superconductor, above-mentioned REBCO superconductor comprise REBCO superconducting layer andBe arranged on the Ag stabilized zone on above-mentioned REBCO superconducting layer.
S200: above-mentioned REBCO superconductor is put in annealing furnace.
S300: will in above-mentioned annealing furnace, vacuumize, while ensureing the annealing of above-mentioned REBCO superconductor at oxygenUnder atmosphere, carry out.
S400: be filled with oxygen in above-mentioned annealing furnace, above-mentioned annealing furnace is provided with pressure regulator valve, by above-mentionedPressure regulator valve regulates the oxygen pressure in above-mentioned annealing furnace, the oxygen pressure in above-mentioned annealing furnace be 1atm withUpper 0.015MPa;
S500: above-mentioned annealing furnace heats up, and is warming up to annealing temperature, and above-mentioned annealing temperature is 500 DEG C, controlsApproximately 5 DEG C/min of heating rate, the 100min that approximately heats up is to above-mentioned annealing temperature.
In S600:S500, reach after 500 DEG C of annealing temperatures, keep annealing temperature constant temperature, constant temperature 5h, makesState the abundant oxygen uptake of REBCO superconductor;
S700: above-mentioned annealing furnace is cooled to room temperature, is cooled to room temperature by 500 DEG C, controls rate of temperature fall0.5℃/min。
S800: take out the above-mentioned REBCO superconductor after oxygen inhalation under pressure annealing, to above-mentioned REBCO superconductionMaterial carries out critical current test.
Embodiment 4
The oxygen inhalation under pressure method for annealing that discloses a kind of REBCO superconductor in embodiment 4, mainly comprisesFollowing steps:
S100: preparation REBCO superconductor, above-mentioned REBCO superconductor comprise REBCO superconducting layer andBe arranged on the Ag stabilized zone on above-mentioned REBCO superconducting layer.
S200: above-mentioned REBCO superconductor is put in annealing furnace.
S300: will in above-mentioned annealing furnace, vacuumize, while ensureing the annealing of above-mentioned REBCO superconductor at oxygenUnder atmosphere, carry out.
S400: be filled with oxygen in above-mentioned annealing furnace, above-mentioned annealing furnace is provided with pressure regulator valve, by above-mentionedPressure regulator valve regulates the oxygen pressure in above-mentioned annealing furnace, the oxygen pressure in above-mentioned annealing furnace be 1atm withUpper 0.02MPa;
S500: above-mentioned annealing furnace heats up, and is warming up to annealing temperature, and above-mentioned annealing temperature is 500 DEG C, controlsApproximately 5 DEG C/min of heating rate, the 100min that approximately heats up is to above-mentioned annealing temperature.
In S600:S500, reach after 500 DEG C of annealing temperatures, keep annealing temperature constant temperature, constant temperature 5h, makesState the abundant oxygen uptake of REBCO superconductor;
S700: above-mentioned annealing furnace is cooled to room temperature, is cooled to room temperature by 500 DEG C, controls rate of temperature fall0.5℃/min。
S800: take out the above-mentioned REBCO superconductor after oxygen inhalation under pressure annealing, to above-mentioned REBCO superconductionMaterial carries out critical current test.
Embodiment 5
The oxygen inhalation under pressure method for annealing that discloses a kind of REBCO superconductor in embodiment 5, mainly comprisesFollowing steps:
S100: preparation REBCO superconductor, above-mentioned REBCO superconductor comprise REBCO superconducting layer andBe arranged on the Ag stabilized zone on above-mentioned REBCO superconducting layer.
S200: above-mentioned REBCO superconductor is put in annealing furnace.
S300: will in above-mentioned annealing furnace, vacuumize, while ensureing the annealing of above-mentioned REBCO superconductor at oxygenUnder atmosphere, carry out.
S400: be filled with oxygen in above-mentioned annealing furnace, above-mentioned annealing furnace is provided with pressure regulator valve, by above-mentionedPressure regulator valve regulates the oxygen pressure in above-mentioned annealing furnace, the oxygen pressure in above-mentioned annealing furnace be 1atm withUpper 0.025MPa;
S500: above-mentioned annealing furnace heats up, and is warming up to annealing temperature, and above-mentioned annealing temperature is 500 DEG C, controlsApproximately 5 DEG C/min of heating rate, the 100min that approximately heats up is to above-mentioned annealing temperature.
In S600:S500, reach after 500 DEG C of annealing temperatures, keep annealing temperature constant temperature, constant temperature 5h, makesState the abundant oxygen uptake of REBCO superconductor;
S700: above-mentioned annealing furnace is cooled to room temperature, is cooled to room temperature by 500 DEG C, controls rate of temperature fall0.5℃/min。
S800: take out the above-mentioned REBCO superconductor after oxygen inhalation under pressure annealing, to above-mentioned REBCO superconductionMaterial carries out critical current test.
Embodiment 6
The oxygen inhalation under pressure method for annealing that discloses a kind of REBCO superconductor in embodiment 6, mainly comprisesFollowing steps:
S100: preparation REBCO superconductor, above-mentioned REBCO superconductor comprise REBCO superconducting layer andBe arranged on the Ag stabilized zone on above-mentioned REBCO superconducting layer.
S200: above-mentioned REBCO superconductor is put in annealing furnace.
S300: will in above-mentioned annealing furnace, vacuumize, while ensureing the annealing of above-mentioned REBCO superconductor at oxygenUnder atmosphere, carry out.
S400: be filled with oxygen in above-mentioned annealing furnace, above-mentioned annealing furnace is provided with pressure regulator valve, by above-mentionedPressure regulator valve regulates the oxygen pressure in above-mentioned annealing furnace, the oxygen pressure in above-mentioned annealing furnace be 1atm withUpper 0.030MPa;
S500: above-mentioned annealing furnace heats up, and is warming up to annealing temperature, and above-mentioned annealing temperature is 500 DEG C, controlsApproximately 5 DEG C/min of heating rate, the 100min that approximately heats up is to above-mentioned annealing temperature.
In S600:S500, reach after 500 DEG C of annealing temperatures, keep annealing temperature constant temperature, constant temperature 5h, makesState the abundant oxygen uptake of REBCO superconductor;
S700: above-mentioned annealing furnace is cooled to room temperature, is cooled to room temperature by 500 DEG C, controls rate of temperature fall0.5℃/min。
S800: take out the above-mentioned REBCO superconductor after oxygen inhalation under pressure annealing, to above-mentioned REBCO superconductionMaterial carries out critical current test.
Embodiment 7
The oxygen inhalation under pressure method for annealing that discloses a kind of REBCO superconductor in embodiment 7, mainly comprisesFollowing steps:
S100: preparation REBCO superconductor, above-mentioned REBCO superconductor comprise REBCO superconducting layer andBe arranged on the Ag stabilized zone on above-mentioned REBCO superconducting layer.
S200: above-mentioned REBCO superconductor is put in annealing furnace.
S300: will in above-mentioned annealing furnace, vacuumize, while ensureing the annealing of above-mentioned REBCO superconductor at oxygenUnder atmosphere, carry out.
S400: be filled with oxygen in above-mentioned annealing furnace, above-mentioned annealing furnace is provided with pressure regulator valve, by above-mentionedPressure regulator valve regulates the oxygen pressure in above-mentioned annealing furnace, the oxygen pressure in above-mentioned annealing furnace be 1atm withUpper 0.015MPa;
S500: above-mentioned annealing furnace heats up, and is warming up to annealing temperature, and above-mentioned annealing temperature is 550 DEG C, controlsApproximately 6 DEG C/min of heating rate.
In S600:S500, reach after 500 DEG C of annealing temperatures, keep annealing temperature constant temperature, constant temperature 6h, makesState the abundant oxygen uptake of REBCO superconductor;
S700: above-mentioned annealing furnace is cooled to room temperature, is cooled to room temperature by 550 DEG C, controls 1 DEG C of rate of temperature fall/min。
S800: take out the above-mentioned REBCO superconductor after oxygen inhalation under pressure annealing, to above-mentioned REBCO superconductionMaterial carries out critical current test.
Embodiment 8
REBCO superconductor after embodiment 8 anneals to oxygen inhalation under pressure in embodiment 1-7 carries out critical electricityCurrent test, critical current test result as shown in fig. 1, within the scope of the above 0-0.015MPa of 1atm,Along with oxygen pressure increases, the critical electric current value of REBCO superconductor is increasing, wherein at 0.015MPaTime reach peak, then along with oxygen pressure increases, the critical electric current value of REBCO superconductor diminishes gradually.
REBCO(REBa2Cu3O7-x, x is 0≤x≤0.6) and superconductor belongs to complicated perovskite structure,Its oxygen content is not 7 under perfect condition conventionally, when oxygen content x gradually changes to 0.6 time by 0, superThe structure of leading material turns to Tetragonal by orthogonal phase transformation, and the superconductivity of material fades away. But oxygen containsAmount is not more high better, and appropriate oxygen defect can be introduced defect in material, plays the order of pinning magnetic flux. Therefore, in above-described embodiment, by adjusting different partials pressure of oxygen, we can well control superconduction materialOxygen content in material, thus realize high critical current.
As shown in fig. 1 for partial pressure of oxygen superconductor in the time of the above 0.015Mpa of 1atm have more suitableOxygen content, thus higher critical current obtained.
The oxygen inhalation under pressure method for annealing of the REBCO superconductor in above-described embodiment, by being adjusted in oxygenOxygen pressure under atmosphere, can increase the diffusion rate of oxygen in superconductor, and superconductor is being moved backIn fire process, oxygen uptake is more abundant, thereby increases the critical electric current value of superconductor, compares existing lehr attendantSkill, can reduce annealing time, thereby enhance productivity.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field can be realized or useThe present invention. To be aobvious and easy for those skilled in the art to the multiple amendment of these embodimentSee, General Principle as defined herein can be in the situation that not departing from the spirit or scope of the present invention,Realize in other embodiments. Therefore, the present invention will can not be restricted to these embodiment shown in this article,But to meet the widest scope consistent with principle disclosed herein and features of novelty.