CN112331435B - Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) Method for regulating and controlling magnetic resistance conversion behavior of composite material - Google Patents
Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) Method for regulating and controlling magnetic resistance conversion behavior of composite material Download PDFInfo
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- 229910003321 CoFe Inorganic materials 0.000 title claims abstract description 44
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 11
- 230000001276 controlling effect Effects 0.000 title claims abstract description 10
- 230000001105 regulatory effect Effects 0.000 title claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 44
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000003825 pressing Methods 0.000 claims abstract description 11
- 238000005303 weighing Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 4
- 239000011812 mixed powder Substances 0.000 claims description 34
- 239000000203 mixture Substances 0.000 claims description 25
- 238000000498 ball milling Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910001566 austenite Inorganic materials 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 230000005294 ferromagnetic effect Effects 0.000 description 10
- 230000000694 effects Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005290 antiferromagnetic effect Effects 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 229910002075 lanthanum strontium manganite Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 230000005641 tunneling Effects 0.000 description 2
- 230000005330 Barkhausen effect Effects 0.000 description 1
- 229910003372 La2/3Sr1/3MnO3 Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Abstract
The invention discloses a Sr 2 FeMoO 6 (1‑x)‑CoFe 2 O 4 (x) Method for regulating and controlling magnetic resistance conversion behavior of composite material, and CoFe 2 O 4 And Sr 2 FeMoO 6 Grinding into powder in agate mortar, and grinding the obtained CoFe 2 O 4 Powder and Sr 2 FeMoO 6 Powder according to Sr 2 FeMoO 6 (1‑x)‑CoFe 2 O 4 (x) Weighing, mixing, grinding and pressing into round slices with diameter of 10mm plus or minus 1mm and thickness of 1mm plus or minus 0.1mm under pressure of 6MPa, wherein x is more than or equal to 0wt% and less than or equal to 55wt%, and H of the composite material is increased along with the increase of x value C The (MR) gradually changes from positive to negative, the magneto-resistance exhibits switching behavior, and as the x value increases, the magneto-resistance switching of the composite material becomes more pronounced. The invention can controllably modulate the magneto-resistance behavior conversion by controlling the specific feeding ratio, and the preparation process is simple and has higher repeatability.
Description
Technical Field
The invention belongs to the technical field of magnetic resistance composite materials, and in particular relates to Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) A method for regulating and controlling the magnetic resistance conversion behavior of a composite material.
Background
In 1991, B.Dieney developed a new approach to the discovery that Barkhausen noise can be effectively suppressed by antiferromagnetic layer exchange coupling meansIn the following, and based on the finding of the multi-layered giant magnetoresistance effect in multi-layered films of repeated simple magnetoresistive structures, a Spin Valve (Spin Valve) structure of four-layered films of ferromagnetic layer/nonmagnetic spacer layer/ferromagnetic layer/antiferromagnetic layer was proposed (diene B, spriosu V S, et al Gaint magnetoresistance in soft ferromagnetic multilayers. Phys. Rev. B. 1991, 43:1297-1300). In 2007, the D.D. Sarma study group passed through a soft ferromagnetic Sr 2 FeMoO 6 Systematic study of samples, in Sr 2 FeMoO 6 Different from the conventional tunneling magnetoresistance effect, namely a novel MR effect similar to a spin valve controlled by grain boundary magnetism is proposed: SVMR effect (Sarma D.D., sugata Ray, et al Intergranular Magnetoresistance in Sr) 2 FeMoO 6 from a Magnetic Tunnel Barrier Mechanism across Grain boundaries. Phys. Rev. Lett. 2007, 98: 157205). In 2012, d.d. Sarma study group in soft ferromagnetic La 2/3 Sr 1/3 MnO 3 Incorporation of hard ferromagnetic insulating material CoFe into (LSMO) grain boundaries 2 O 4 Modification of (CFO), in (LSMO) 1-x -(CFO) x (0.ltoreq.x.ltoreq.0.5) based on SVMR observed in the composite system, H is determined by varying the value of x C The (MR) value may gradually change from a positive value to a negative value (and vice versa): namely, a magneto-resistive switching behavior (Anil Kumar 1P. And Sara D.D. Effect of "bipolar-biasing" on the tunability of tunneling magnetoresistance in transition metal oxide systems, appl. Phys. Lett. 2012, 100:26407) occurs. In 2015, the subject group of G.Muscas was also in soft ferromagnetic La 0.67 Ca 0.33 MnO 3 (LCMO) -hard ferromagnetic CoFe 2 O 4 After SVMR behavior was observed in the (CFO) composite, magneto-resistive switching behavior was also found by varying the temperature of the test (Muscas G., anil Kumar P., designing new ferrite/manganite nanocomposites. Nanoscales.2015, 8 (4), 2081-2089).
But to date, in relation to the soft ferromagnetic Sr 2 FeMoO 6 Incorporation of hard ferromagnetic CoFe in (SFMO) 2 O 4 The study of whether the magneto-resistance conversion behavior occurs after (CFO) has not been reported in the literature, and therefore the system of the SFMO-CFO composite materialThere is a certain significance in research.
Disclosure of Invention
The invention solves the technical problem of providing a Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) Method for regulating and controlling magnetic resistance conversion behavior of composite material, and single-phase Sr formed by firing under specific conditions 2 FeMoO 6 With CoFe 2 O 4 Grinding round slices into powder, and mixing the powder with Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) (x=0wt%, 10wt%, 28wt%, 55wt%) weighing, mixing, grinding and pressing into round sheet, and can clearly be used in Sr after test 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) A transition in respect of the magneto-resistive behaviour is observed in the composite system. The invention can controllably modulate the magnetic resistance behavior conversion of the composite material by controlling the specific feeding quality ratio, and the preparation process is simple and has higher repeatability.
The invention adopts the following technical proposal to solve the technical problems that Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) The method for regulating and controlling the magnetic resistance conversion behavior of the composite material is characterized by comprising the following specific processes: coFe is to be CoFe 2 O 4 And Sr 2 FeMoO 6 Grinding into powder in agate mortar, and grinding the obtained CoFe 2 O 4 Powder and Sr 2 FeMoO 6 Powder according to Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) Weighing, mixing, grinding and pressing into round slices with diameter of 10mm plus or minus 1mm and thickness of 1mm plus or minus 0.1mm under pressure of 6MPa, wherein x is more than or equal to 0wt% and less than or equal to 55wt%, and H of the composite material is increased along with the increase of x value C The (MR) gradually changes from positive to negative, the magneto-resistance exhibits switching behavior, and as the x value increases, the magneto-resistance switching of the composite material becomes more pronounced.
Further defined, the CoFe 2 O 4 The specific preparation process of (2) is as follows:
step A1: mixing CoO powder with purity of 99% and nano magnetic iron oxide gamma-Fe with purity of 99.5% 2 O 3 Weighing and mixing the powder according to a molar ratio of 1:1;
step A2: adding alcohol into the mixed powder obtained in the step A1, placing the mixed powder into a ball milling tank for ball milling for 10-24 hours to uniformly mix the powder, and then drying to obtain mixed powder;
step A3: pressing the mixed powder obtained in the step A2 into a round sheet with the diameter of 10mm plus or minus 1mm and the thickness of 1mm plus or minus 0.1mm by using the pressure of 4 MPa;
step A4: placing the mixed powder obtained in the step A2 into a magnetic boat, embedding the round flake obtained in the step A3 into the mixed powder in the magnetic boat, and then adding the mixed powder into the magnetic boat according to the volume percentage of 1%H 2 Heating to 510 ℃ under the mixed atmosphere of Ar with concentration of 99 percent, preserving heat for 0.5h, and finally cooling to room temperature along with a furnace to obtain CoFe 2 O 4 。
Further defined, the Sr 2 FeMoO 6 The specific preparation process of (2) is as follows:
step B1: according to Sr 2 FeMoO 6 Respectively weighing SrCO with purity of 99.5% after drying treatment 3 Powder and Fe with purity of 99.9% 2 O 3 Powder and MoO with 99.9% purity 3 Adding alcohol into a mixture of the three powders, placing the mixture into a ball milling tank for ball milling for 10-24 hours to uniformly mix the powders, and then drying to obtain mixed powder;
step B2: presintering the mixed powder obtained in the step B1 in an air atmosphere at 900 ℃ for 10 hours, adding alcohol into the presintered mixed powder, putting the mixture into a ball milling tank, ball milling for 10-24 hours again, and drying to obtain a powder mixture;
step B3: pressing the powder mixture obtained in the step B2 into round slices with the diameter of 10mm plus or minus 1mm and the thickness of 1mm plus or minus 0.1mm by using the pressure of 4 MPa;
step B4: placing the powder mixture obtained in the step B2 into a magnetic boat, embedding the round flake obtained in the step B3 into the mixed powder in the magnetic boat, and then adding the mixed powder into the magnetic boat according to the volume percentage of 3%H 2 Heating to 1300 ℃ under the mixed atmosphere of/97 percent Ar, preserving heat for 10 hours, and finally cooling to room temperature along with the furnace to obtain Sr 2 FeMoO 6 。
The invention is characterized in thatCompared with the prior art, the method has the following beneficial effects: the synthesis process and the required equipment are simple, and the method only adopts the traditional solid phase reaction method to prepare the catalyst according to Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) (x=0wt%, 10wt%, 28wt%, 55wt%) weighing, mixing, grinding and pressing into round sheet, and after test, the sheet can be clearly used as Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) A transition in respect of the magneto-resistive behaviour is observed in the composite system. The invention can controllably modulate the magneto-resistance behavior conversion by controlling the specific feeding quality ratio, and the preparation process is simple and has higher repeatability.
Drawings
FIG. 1 shows the Sr synthesized according to the present invention 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) (x=0 wt%, 10wt%, 28wt%, 55 wt%) XRD pattern of the composite system;
FIG. 2 is a synthetic Sr of the present invention 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) Hysteresis spin (M-H) curve (10K) of (x=0 wt%, 10wt%, 28wt%, 55 wt%) composite system;
FIG. 3 shows the Sr synthesized according to the present invention 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) (x=0 wt%, 10wt%, 28wt%, 55 wt%) of the (MR-H) curve (10K) of the composite system.
Detailed Description
The above-described matters of the present invention will be described in further detail by way of examples, but it should not be construed that the scope of the above-described subject matter of the present invention is limited to the following examples, and all techniques realized based on the above-described matters of the present invention are within the scope of the present invention.
Examples
CoFe 2 O 4 Is prepared from the following steps:
step A1: mixing CoO powder with purity of 99% and nano magnetic iron oxide gamma-Fe with purity of 99.5% 2 O 3 Weighing and mixing the powder according to a molar ratio of 1:1;
step A2: adding alcohol into the mixed powder obtained in the step A1, placing the mixed powder into a ball milling tank for ball milling for 10-24 hours to uniformly mix the powder, and then drying to obtain mixed powder;
step A3: pressing the mixed powder obtained in the step A2 into a round sheet with the diameter of 10mm plus or minus 1mm and the thickness of 1mm plus or minus 0.1mm by using the pressure of 4 MPa;
step A4: placing the mixed powder obtained in the step A2 into a magnetic boat, embedding the round flake obtained in the step A3 into the mixed powder in the magnetic boat, and then adding the mixed powder into the magnetic boat according to the volume percentage of 1%H 2 Heating to 510 ℃ under the mixed atmosphere of Ar with concentration of 99 percent, preserving heat for 0.5h, and finally cooling to room temperature along with a furnace to obtain CoFe 2 O 4 。
Sr 2 FeMoO 6 Is prepared from the following steps:
step B1: according to Sr 2 FeMoO 6 Respectively weighing SrCO with purity of 99.5% after drying treatment 3 Powder and Fe with purity of 99.9% 2 O 3 Powder and MoO with 99.9% purity 3 Adding alcohol into a mixture of the three powders, placing the mixture into a ball milling tank for ball milling for 10-24 hours to uniformly mix the powders, and then drying to obtain mixed powder;
step B2: presintering the mixed powder obtained in the step B1 in an air atmosphere at 900 ℃ for 10 hours, adding alcohol into the presintered mixed powder, putting the mixture into a ball milling tank, ball milling for 10-24 hours again, and drying to obtain a powder mixture;
step B3: pressing the powder mixture obtained in the step B2 into round slices with the diameter of 10mm plus or minus 1mm and the thickness of 1mm plus or minus 0.1mm by using the pressure of 4 MPa;
step B4: placing the powder mixture obtained in the step B2 into a magnetic boat, embedding the round sheet obtained in the step B3 into the powder mixture in the magnetic boat, and then performing a volume percentage 3%H 2 Heating to 1300 ℃ under the mixed atmosphere of/97 percent Ar, preserving heat for 10 hours, and finally cooling to room temperature along with the furnace to obtain Sr 2 FeMoO 6 。
Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) Preparation of the composite material:
step C1: the CoFe obtained in the step A4 is processed 2 O 4 And Sr obtained in the step B4 2 FeMoO 6 Respectively arranged atGrinding the materials into powder in an agate mortar;
step C2: the powder obtained in C1 is prepared according to Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) The feed ratios (x=0 wt%, 10wt%, 28wt%, 55 wt%) were weighed, mixed, ground and pressed into round flakes of 10mm±1mm diameter and 1mm±0.1mm thickness, respectively, under a pressure of 6 MPa.
Test results:
FIG. 1 is Sr of the example 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) (x=0 wt%, 10wt%, 28wt%, 55 wt%) XRD pattern of the composite system, verifying the presence of Sr in the composite 2 FeMoO 6 And CoFe 2 O 4 Two sets of diffraction peaks, and CoFe as the x value increases 2 O 4 The diffraction peak intensity of (2) is gradually enhanced. The invention can prepare the composite material Sr by using the simple and easy experimental scheme 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) A system.
FIG. 2 is Sr of the embodiment 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) (x=0 wt%, 10wt%, 28wt%, 55 wt%) hysteresis (M-H) curve (10K) of the composite system. The M-H curve at 10K shows the synthesized Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) H of composite material C 101Oe, 192Oe, 384Oe and 2087Oe, respectively, it can be seen that Sr increases with increasing x value 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) Coercive field (H) of the composite material C ) And become larger and larger.
FIG. 3 is Sr of the embodiment 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) (x=0 wt%, 10wt%, 28wt%, 55 wt%) MR-H curve (10K) of the composite system. The MR-H curve at 10K shows the magnetic field value H corresponding to the maximum value of the reluctance in the insets of the a and b plots when the magnetic field is swept from-2.5T to 2.5T (both shown by the diagonal upward arrow in the a, b, c, d plot) C (MR) (dashed line position in the inset) is 1000Oe, 600Oe, respectively. Magnetic field value H corresponding to the maximum value of magnetic resistance in the insets of c and d C (MR) (dashed line position in the inset) is-316 Oe, -1010Oe, respectively. From the four dataAs can be seen from comparison of the values, as the value of x increases, H of the composite material C From this result, it can be clearly observed that the magneto-resistance exhibits a switching behavior from a positive value to a negative value, and that the magneto-resistance switching of the composite material is more pronounced as the value of x increases.
While the basic principles, principal features and advantages of the present invention have been described in the foregoing examples, it will be appreciated by those skilled in the art that the present invention is not limited by the foregoing examples, but is merely illustrative of the principles of the invention, and various changes and modifications can be made without departing from the scope of the invention, which is defined by the appended claims.
Claims (1)
1.Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) The method for regulating and controlling the magnetic resistance conversion behavior of the composite material is characterized by comprising the following specific processes: coFe is to be CoFe 2 O 4 And Sr 2 FeMoO 6 Grinding into powder in agate mortar, and grinding the obtained CoFe 2 O 4 Powder and Sr 2 FeMoO 6 Powder according to Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) Weighing, mixing, grinding and pressing under 6MPa to obtain round sheet with diameter of 10 mm+ -1 mm and thickness of 1 mm+ -0.1 mm, wherein x is more than or equal to 0wt% and less than or equal to 55wt%, and H is the composite material with the increase of x value C (MR) gradually changes from positive to negative, the magneto-resistance exhibits switching behavior, and as the value of x increases, the magneto-resistance switching of the composite material becomes more pronounced;
the CoFe 2 O 4 The specific preparation process of (2) is as follows:
step A1: mixing CoO powder with purity of 99% and nano magnetic iron oxide gamma-Fe with purity of 99.5% 2 O 3 Weighing and mixing the powder according to a molar ratio of 1:1;
step A2: adding alcohol into the mixed powder obtained in the step A1, placing the mixed powder into a ball milling tank for ball milling for 10-24 hours to uniformly mix the powder, and then drying to obtain mixed powder;
step A3: pressing the mixed powder obtained in the step A2 into a round sheet with the diameter of 10mm plus or minus 1mm and the thickness of 1mm plus or minus 0.1mm by using the pressure of 4 MPa;
step A4: placing the mixed powder obtained in the step A2 into a magnetic boat, embedding the round flake obtained in the step A3 into the mixed powder in the magnetic boat, and then adding the mixed powder into the magnetic boat according to the volume percentage of 1%H 2 Heating to 510 ℃ under the mixed atmosphere of Ar with concentration of 99 percent, preserving heat for 0.5h, and finally cooling to room temperature along with a furnace to obtain CoFe 2 O 4 ;
The Sr is 2 FeMoO 6 The specific preparation process of (2) is as follows:
step B1: according to Sr 2 FeMoO 6 Respectively weighing SrCO with purity of 99.5% after drying treatment 3 Powder and Fe with purity of 99.9% 2 O 3 Powder and MoO with 99.9% purity 3 Adding alcohol into a mixture of the three powders, placing the mixture into a ball milling tank for ball milling for 10-24 hours to uniformly mix the powders, and then drying to obtain mixed powder;
step B2: presintering the mixed powder obtained in the step B1 in an air atmosphere at 900 ℃ for 10 hours, adding alcohol into the presintered mixed powder, putting the mixture into a ball milling tank, ball milling for 10-24 hours again, and drying to obtain a powder mixture;
step B3: pressing the powder mixture obtained in the step B2 into round slices with the diameter of 10mm plus or minus 1mm and the thickness of 1mm plus or minus 0.1mm by using the pressure of 4 MPa;
step B4: placing the powder mixture obtained in the step B2 into a magnetic boat, embedding the round flake obtained in the step B3 into the mixed powder in the magnetic boat, and then adding the mixed powder into the magnetic boat according to the volume percentage of 3%H 2 Heating to 1300 ℃ under the mixed atmosphere of/97 percent Ar, preserving heat for 10 hours, and finally cooling to room temperature along with the furnace to obtain Sr 2 FeMoO 6 。
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