CN102633495A - Preparation method of room-temperature ferromagnetic Sr2FemMonO6 ceramic - Google Patents

Preparation method of room-temperature ferromagnetic Sr2FemMonO6 ceramic Download PDF

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CN102633495A
CN102633495A CN2012101062129A CN201210106212A CN102633495A CN 102633495 A CN102633495 A CN 102633495A CN 2012101062129 A CN2012101062129 A CN 2012101062129A CN 201210106212 A CN201210106212 A CN 201210106212A CN 102633495 A CN102633495 A CN 102633495A
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preparation
thin slice
room
pottery
temperature
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CN102633495B (en
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张善涛
王金凤
基维静
顾正彬
周健
陈延彬
姚淑华
陈延峰
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Nanjing University
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Nanjing University
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Abstract

The invention discloses a preparation method of room-temperature ferromagnetic Sr2FemMonO6 ceramic, wherein m is 10/9, n is 8/9 or m is 7/6 and n is 5/6. The preparation method comprises the following steps of: carrying out ball-milling, pre-sintering and ball-milling on mixture of powder by utilizing SrCO3, Fe2O3 and MoO3 powder, tabletting the obtained powder mixture which is uniformly mixed and then sintering the powder mixture under N2 atmosphere, wherein the sintering temperature is 1160 DEG C and the sintering time is 40 hours. Single-phase Sr2Fe10/9Mo8/9O6 and Sr2Fe7/6Mo5/6O6 ceramics with high qualities are obtained by adopting the preparation method disclosed by the invention. The ceramics have ferromagnetic curie temperature higher than the room temperature; and the required device and preparation process for preparation of the ceramics are simple without H2 atmosphere, and the preparation condition is easier.

Description

Room-temperature ferromagnetic Sr 2Fe mMo nO 6The preparation method of pottery
Technical field
The present invention relates to a kind of preparation method of pottery.
Background technology
Sr 2FeMoO 6Type double-perovskite oxide material has the ferromagnetic Curie temperature (T that is higher than room temperature (300K) c~420K), higher spin polarizability and bigger magneto-resistor, therefore in much working in room temperature or above device, very important application prospect is arranged.While Sr 2FeMoO 6Sections magnetic double-perovskite oxide compound also is the various basic physical problems of research; Important materials like coexistence, coupling and competitive relation complicated between the spin in the strong correlation electron system, track, electric charge and the lattice degree of freedom; In these years, the research about ferromegnetism double-perovskite oxide material has obtained good development.But the preparation condition of sample is comparatively harsh, and high-quality pottery and film sample can only be at H 2Obtain under the atmosphere with conditions such as certain sintering temperature and sintering time under obtain, and these not only can cause cost and the increases of testing danger, also can reduce the repeatability of specimen preparation and character thereof, for example, the Sr of various different structures 2FeMoO 3Report is all arranged.
So, need a kind of new preparation method to address the above problem.
Summary of the invention
Goal of the invention: the objective of the invention is to prior art Sr 2FeMoO 6The preparation condition of type double-perovskite oxide material is harsh, and high-quality pottery and film sample can only be at H 2The defective that obtains under the atmosphere provides a kind of room-temperature ferromagnetic Sr 2Fe mMo nO 6The preparation method of pottery is to address the above problem.
Technical scheme: for realizing foregoing invention purpose, room-temperature ferromagnetic Sr of the present invention 2Fe mMo nO 6The preparation method of pottery can adopt following technical scheme:
A kind of room-temperature ferromagnetic Sr 2Fe mMo nO 6The preparation method of pottery, m=10/9 wherein, n=8/9 or m=7/6, n=5/6 may further comprise the steps:
(1), according to chemical formula Sr 2Fe mMo nO 6, weighing is through the SrCO of drying treatment 3, Fe 2O 3And MoO 3Powder;
(2), with SrCO 3, Fe 2O 3And MoO 3Powder is through ball-milling processing, pre-burning for the first time, ball-milling processing makes three kinds of powder even for the second time;
(3), the powdered mixture that mixes is pressed into thin slice;
(4), will the powdered mixture of step (2) gained put into crucible, put into the thin slice of step (3) gained again, and cover said thin slice with the powdered mixture of step (2) gained, said thin slice is embedded among the powdered mixture of step (2) gained;
The crucible that (5) thin slice will be housed is put into retort furnace, and feeds mobile N 2, be warmed up to 1160 ℃ of sintering temperatures, make thin slice 1160 ℃ of sintering 40 hours, obtain Sr 2Fe mMo nO 6Pottery.
Beneficial effect: compared with prior art, room-temperature ferromagnetic Sr of the present invention 2Fe mMo nO 6The preparation method of pottery is at N 2Can prepare high quality, monophasic Sr under the atmosphere 2Fe 10/9Mo 8/9O 6And Sr 2Fe 7/6Mo 5/6O 6Pottery, these potteries have the ferromagnetic Curie temperature that is higher than room temperature, and it is simple to prepare these potteries required equipment and preparation process, need not H 2Atmosphere, preparation condition is loose.
Description of drawings
Fig. 1 is the Sr that specific embodiment 1 prepares 2Fe 10/9Mo 8/9O 6The Sr for preparing with specific embodiment 2 2Fe 7/6Mo 5/6O 6The x ray diffraction spectra (XRD) of pottery;
Fig. 2 is the Sr that specific embodiment 1 prepares 2Fe 10/9Mo 8/9O 6The Sr for preparing with specific embodiment 2 2Fe 7/6Mo 5/6O 6The room temperature magnetic hysteresis loop of pottery;
Fig. 3 is the Sr that specific embodiment 1 prepares 2Fe 10/9Mo 8/9O 6The Sr that pottery and specific embodiment 2 prepare 2Fe 7/6Mo 5/6O 6The specific magnetising moment-the temperature curve of pottery.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment; Further illustrate the present invention; Should understand these embodiment only be used to the present invention is described and be not used in the restriction scope of the present invention; After having read the present invention, those skilled in the art all fall within the application's accompanying claims institute restricted portion to the modification of the various equivalent form of values of the present invention.
Specific embodiment 1:
(1), according to chemical formula Sr 2Fe 10/9Mo 8/9O 6, weighing through the purity of drying treatment more than or equal to 99.0% SrCO 3, Fe 2O 3And MoO 3Powder adds alcohol in the mixture of three kinds of powder, ball-milling processing (320 rev/mins, 24 hours) makes powder even then;
(2), the powdered mixture of step (1) gained carried out drying treatment after, grinds with mortar and to make it evenly, and in 800 ℃, pre-burning is 5 hours in the air, and then grind with mortar and to make it even;
(3), in the powdered mixture of step (2) gained, add alcohol, ball-milling processing (320 rev/mins, 24 hours) makes it further to mix then, and drying treatment;
(4), the powdered mixture with step (3) gained of the pressure handle of 20MPa is pressed into thin slice.Thin slice is a rectangle, and length is 10mm ± 1mm, and width is 5mm ± 1mm, and the thickness of thin slice is 1mm ± 0.1mm, with the electronic transport character detection of convenient pottery;
(5), the powdered mixture of step (3) gained is put into crucible, put into thin slice again, and, thin slice is embedded among the powdered mixture of step (3) gained with the powdered mixture cover sheet of step (3) gained;
(6), crucible that thin slice will be housed is put into retort furnace, and is fed mobile N 2, temperature rise rate is controlled at 3 ℃/minute.In temperature-rise period, temperature is incubated 30 minutes in the time of 400 ℃, and then is warmed up to 1160 ℃ of sintering temperatures.Make thin slice 1160 ℃ of sintering 40 hours, obtain corresponding pottery.
Specific embodiment 2:
(1), according to chemical formula Sr 2Fe 7/6Mo 5/6O 6, weighing through drying treatment purity more than or equal to 99.0% SrCO 3, Fe 2O 3And MoO 3Powder adds alcohol in the mixture of three kinds of powder, ball-milling processing (320 rev/mins, 24 hours) makes powder even then;
(2), the powdered mixture of step (1) gained carried out drying treatment after, grinds with mortar and to make it evenly, and in 800 ℃, pre-burning is 5 hours in the air, and then grind with mortar and to make it even;
(3), in the powdered mixture of step (2) gained, add alcohol, ball-milling processing (320 rev/mins, 24 hours) makes it further to mix then, and drying treatment;
(4), the pressure with 20MPa is pressed into thin slice to the powdered mixture of step (3) gained.Thin slice is a rectangle, and length is 10mm ± 1mm, and width is 5mm ± 1mm, and the thickness of thin slice is 1mm ± 0.1mm, with the electronic transport character detection of convenient pottery;
(5), the powdered mixture of step (3) gained is put into crucible, put into thin slice again, and, thin slice is embedded among the powdered mixture of step (3) gained with the powdered mixture cover sheet of step (3) gained.
(6), crucible that thin slice will be housed is put into retort furnace, and is fed mobile N 2, temperature rise rate is controlled at 3 ℃/minute.In temperature-rise period, temperature is incubated 30 minutes, and then is warmed up to sintering temperature in the time of 400 ℃.Make thin slice 1160 ℃ of sintering 40 hours, obtain corresponding pottery.
Test result:
Fig. 1 is the Sr that specific embodiment 1 prepares 2Fe 10/9Mo 8/9O 6The Sr that pottery and specific embodiment 2 prepare 2Fe 7/6Mo 5/6O 6The x ray diffraction spectra (XRD) of pottery, it explains that the pottery for preparing under this condition is monophasic and do not have other dephasigns.
Fig. 2 is the Sr that specific embodiment 1 prepares 2Fe 10/9Mo 8/9O 6The Sr that pottery and specific embodiment 2 prepare 2Fe 7/6Mo 5/6O 6The room temperature magnetic hysteresis loop of pottery, Sr 2Fe 10/9Mo 8/9O 6The saturation magnetization and the residual magnetization of pottery are respectively 9.62emu/g and 0.12emu/g, and Sr 2Fe 7/6Mo 5/6O 6Saturation magnetization and residual magnetization be respectively 4.07emu/g and 0.04emu/g.Its magnetic reduces along with the increase of Fe/Mo ratio.This be since Fe/Mo than greater than after 1, the antiferromagnetic coupling between the adjacent Fe ion strengthens, thereby has reduced the macroscopic ferromegnetism.
Fig. 3 is the Sr that specific embodiment 1 prepares 2Fe 10/9Mo 8/9O 6The Sr that pottery and specific embodiment 2 prepare 2Fe 7/6Mo 5/6O 6The specific magnetising moment-the temperature curve of pottery, externally-applied magnetic field 200 oersteds during test.As can be seen from Figure 3, these ceramic ferromagnetic Curie temperatures are respectively 385K and 380K.
As stated, adopt Sr of the present invention 2Fe mMo nO 6The preparation method of pottery can be at N 2Prepare high quality, monophasic Sr under the atmosphere 2Fe 10/9Mo 8/9O 6Pottery and Sr 2Fe 7/6Mo 5/6O 6Pottery, these potteries have the ferromagnetic Curie temperature that is higher than room temperature, and it is simple to prepare these potteries required equipment and preparation process, need not H 2Atmosphere, preparation condition is loose.

Claims (10)

1. room-temperature ferromagnetic Sr 2Fe mMo nO 6The preparation method of pottery is characterized in that, m=10/9 wherein, and n=8/9 or m=7/6, n=5/6 may further comprise the steps:
(1), according to chemical formula Sr 2Fe mMo nO 6, weighing is through the SrCO of drying treatment 3, Fe 2O 3And MoO 3Powder;
(2), with SrCO 3, Fe 2O 3And MoO 3Powder is through ball-milling processing, pre-burning for the first time, ball-milling processing makes three kinds of powder even for the second time;
(3), the powdered mixture that mixes is pressed into thin slice;
(4), will the powdered mixture of step (2) gained put into crucible, put into the thin slice of step (3) gained again, and cover said thin slice with the powdered mixture of step (2) gained, said thin slice is embedded among the powdered mixture of step (2) gained;
The crucible that (5) thin slice will be housed is put into retort furnace, and feeds mobile N 2, be warmed up to 1160 ℃ of sintering temperatures, make thin slice 1160 ℃ of sintering 40 hours, obtain Sr 2Fe mMo nO 6Pottery.
2. room-temperature ferromagnetic Sr as claimed in claim 1 2Fe mMo nO 6The preparation method of stupalith is characterized in that, the SrCO described in the step (1) 3, Fe 2O 3And MoO 3The purity of powder is more than or equal to 99.0%.
3. room-temperature ferromagnetic Sr as claimed in claim 1 2Fe mMo nO 6The preparation method of pottery is characterized in that, the first time described in the step (2), ball-milling processing may further comprise the steps: in the mixture of three kinds of powder, add alcohol, make three kinds of powder even with ball-milling processing.
4. room-temperature ferromagnetic Sr as claimed in claim 1 2Fe mMo nO 6The preparation method of pottery; It is characterized in that; Pre-burning may further comprise the steps described in the step (2): after the powdered mixture that the first time, ball-milling processing obtained is carried out drying treatment; Make it to mix with the mortar grinding, pre-burning is 5 hours in 800 ℃ air, and then makes it to mix with the mortar grinding.
5. room-temperature ferromagnetic Sr as claimed in claim 1 2Fe mMo nO 6The preparation method of pottery is characterized in that, the second time described in the step (2), ball-milling processing may further comprise the steps: add alcohol in the powdered mixture that after pre-burning, obtains, ball-milling processing mixes powdered mixture then, and carries out drying treatment.
6. room-temperature ferromagnetic Sr as claimed in claim 1 2Fe mMo nO 6The preparation method of pottery is characterized in that, thin slice described in the step (3) is the thin slice that the pressure with 20Mpa is pressed into the powdered mixture that mixes.
7. room-temperature ferromagnetic Sr as claimed in claim 3 2Fe mMo nO 6The preparation method of pottery is characterized in that, the first time described in the step (2), ball-milling processing was under 320 rev/mins condition, to handle 24 hours.
8. room-temperature ferromagnetic Sr as claimed in claim 4 2Fe mMo nO 6The preparation method of pottery is characterized in that, the second time described in the step (2), ball-milling processing was under 320 rev/mins condition, to handle 24 hours.
9. room-temperature ferromagnetic Sr as claimed in claim 1 2Fe mMo nO 6The pottery the preparation method, it is characterized in that, in the step (5) from the room temperature to the sintering temperature 1160 ℃ temperature rise rate be controlled at 3 ℃/minute, in temperature-rise period, temperature is incubated 30 minutes in the time of 400 ℃, and then is warmed up to 1160 ℃ of sintering temperatures.
10. room-temperature ferromagnetic Sr as claimed in claim 1 2Fe mMo nO 6The preparation method of stupalith is characterized in that, the thin slice described in the step (4) is a rectangle, and the length of said thin slice is 10mm ± 1mm, and the width of said thin slice is 5mm ± 1mm, and the thickness of said thin slice is 1mm ± 0.1mm.
CN201210106212.9A 2012-04-11 2012-04-11 Preparation method of room-temperature ferromagnetic Sr2FemMonO6 ceramic Expired - Fee Related CN102633495B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103193487A (en) * 2013-04-22 2013-07-10 南京大学 Method for quantitatively controlling B-position antiposition defect concentration of Sr2FeMoO6 ceramic
CN103342551A (en) * 2013-06-28 2013-10-09 南京大学 Preparation methods of room-temperature ferromagnetic Sr3FeCrMoO9 ceramic and film
CN104108924A (en) * 2014-05-19 2014-10-22 华北水利水电大学 Material having ferrimagnetism and preparation method thereof
CN107473742A (en) * 2017-09-08 2017-12-15 河南师范大学 A kind of single-phase double-perovskite Sr of high quality2FeMoO6The preparation method of ceramics
CN112331435A (en) * 2020-10-09 2021-02-05 河南师范大学 Sr2FeMoO6(1-x)-CoFe2O4(x) Method for regulating and controlling magneto-resistive switching behavior of composite material

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CN102351524A (en) * 2011-06-22 2012-02-15 南京大学 Preparation method for high purity single-phase Sr2FeMoO6

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CN102074713A (en) * 2010-12-17 2011-05-25 天津大学 Anode material for solid oxide fuel cell, preparation method thereof and fuel cell
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103193487A (en) * 2013-04-22 2013-07-10 南京大学 Method for quantitatively controlling B-position antiposition defect concentration of Sr2FeMoO6 ceramic
CN103342551A (en) * 2013-06-28 2013-10-09 南京大学 Preparation methods of room-temperature ferromagnetic Sr3FeCrMoO9 ceramic and film
CN104108924A (en) * 2014-05-19 2014-10-22 华北水利水电大学 Material having ferrimagnetism and preparation method thereof
CN107473742A (en) * 2017-09-08 2017-12-15 河南师范大学 A kind of single-phase double-perovskite Sr of high quality2FeMoO6The preparation method of ceramics
CN107473742B (en) * 2017-09-08 2020-07-17 河南师范大学 High-quality single-phase double perovskite Sr2FeMoO6Method for producing ceramic
CN112331435A (en) * 2020-10-09 2021-02-05 河南师范大学 Sr2FeMoO6(1-x)-CoFe2O4(x) Method for regulating and controlling magneto-resistive switching behavior of composite material
CN112331435B (en) * 2020-10-09 2024-01-19 河南师范大学 Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) Method for regulating and controlling magnetic resistance conversion behavior of composite material

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