CN102351524A - Preparation method for high purity single-phase Sr2FeMoO6 - Google Patents
Preparation method for high purity single-phase Sr2FeMoO6 Download PDFInfo
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- CN102351524A CN102351524A CN2011101689821A CN201110168982A CN102351524A CN 102351524 A CN102351524 A CN 102351524A CN 2011101689821 A CN2011101689821 A CN 2011101689821A CN 201110168982 A CN201110168982 A CN 201110168982A CN 102351524 A CN102351524 A CN 102351524A
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Abstract
Provided is a preparation method for high purity single-phase Sr2FeMoO6. The method comprises the following steps: step 1, putting SrCO3, Fe2O3 and MoO3 with a purity greater than analytical purity in a drying oven for drying, preparing desired components based on the stoichiometric formula of Sr2FeMoO6, fully grinding the components to uniformly mixing the components, putting the ground components in a high temperature sintering furnace for pre-sintering with a sintering temperature being 900 +- 20 DEG C and sintering time being 10 +- 1 h, subjecting carbonate to complete decomposition, and carrying out a preliminary reaction to obtain a sample; step 2, fully grinding and tabletting the pre-sintered sample with grinding time being 2.5 to 4 h and pressure for tabletting being 14 to 18 MPa, carrying out primary high temperature sintering in an mixed atmosphere of H2/Ar, wherein, the proportion of H2/Ar mixed gas is 4-6% v/v, the flow of H2/Ar mixed gas is 20 +- 2 ml/min, sintering temperature is 1280 +- 10 DEG C, and sintering time is 5 +- 1 h, and allowing furnace temperature to naturally decrease after the primary high temperature sintering; repeating step 2 twice to three times.
Description
One, technical field
The field is new function material and preparation method thereof under the present invention.
Two, background technology
In recent years, the research of magneticsubstance has obtained developing rapidly.Magneticsubstance is closely related with the every aspect of informationization, robotization, electromechanical integration, national defence, national economy.Utilize the magnetic resistance material source of present human scientific-technical progress especially of the magnetic effect of resistance.Magneto-resistance effect is to find by Britain physicist William thomson that it can be ignored, and was then apparent in view in semi-conductor in metal in 1857.(magneto-resistance, MR) effect is exactly the phenomenon that changes under the effect of resistivity outside magnetic field of material to magneto-resistor.Albert Fert and Peter Gr ü nberg have shared Nobel Prize in physics in 2007 because of finding giant magnetoresistance effect.Because the widespread use of magnetic resistance material, international and domestic scholar has carried out broad research, has started the upsurge of functional materials research, and the influential international literature of delivering has: 1) Science 309 (2005) 1688; 2) Nature 458 (2009) 489; 3) Science 309 (2005) 257; 4) Nature 457 (2009) 1112; 5) Science 306 (2004) 63; 6) Science 305 (2004) 646; 7) Science 296 (2002) 2003; 8) Science 294 (2001) 1488; 9) Science 291 (2001) 854; 10) Nature Materials 10 (2011) 347; 11) Advanced Materials 23 (2011) 1371.
Huge magnetoresistance material Sr
2FeMoO
6Be that people such as Japanese scientist K.-I.Kobayashi in 1998 find that its international literature of delivering is: Nature 395 (1998) 677. Fig. 2 are Sr
2FeMoO
6The primitive unit cell synoptic diagram.Sr
2FeMoO
6Be typical double-perovskite type structure, spacer is I4/m, and the character constant does
Its Tc is (about 420K) on room temperature, and the magneto-resistance effect when 300K, 7T is up to 10%.Therefore, this material is regarded as one of most possible magnetic resistance material of at room temperature realizing application immediately and receives much concern.
Sr
2FeMoO
6Since finding, just received widely and paying close attention to, researcher becomes phase condition, microstructure, transport property to it, and extensive and deep research has been carried out in magnetic interaction etc.But because pure phase Sr
2FeMoO
6Synthesis condition is quite harsh, causes the preparation of high-purity single-phase sample to become a present bottleneck.
Three, summary of the invention
The objective of the invention is to improve Sr
2FeMoO
6The preparation method, the high-purity single-phase Sr of a kind of simple preparation is proposed
2FeMoO
6Method; The sample that this method is prepared, not only purity is high, and the sample that magneto-resistance effect is prepared than traditional technology significantly improves.
Technical scheme of the present invention is: high-purity single-phase Sr
2FeMoO
6The preparation method, it is characterized in that adopting following steps:
Step 1: with the SrCO more than the analytical pure
3(purity>=99.0wt%), Fe
2O
3(purity>=99.0wt%), MoO
3(purity>=99.5wt%) is placed on and carries out drying in the baking oven, then according to Sr
2FeMoO
6Stoichiometric equation prepare required composition, fully grind it mixed, place the high temperature sintering furnace pre-burning, sintering temperature is 900 ± 20 ℃, sintering time is 10 ± 1h; Initial reaction obtains sample to make carbonate decompose also fully;
Step 2: with the sample of pre-burning fully grind, compressing tablet, milling time is 2.5-4h, pressure is 14-18Mpa during compressing tablet; At H
2Carry out the high temperature sintering first time in the/Ar mixed atmosphere; H
2The ratio of/Ar mixed gas is 4-6%v/v, and flow is 20 ± 2ml/min; Sintering temperature is 1280 ± 10 ℃, and sintering time is 5 ± 1h, and behind the high temperature sintering, furnace temperature is lowered the temperature naturally;
Step 3: the sample behind the general's high temperature sintering first time grinds, compressing tablet, and milling time is 1.5-2h, and pressure is 14-18Mpa during compressing tablet; Then at H
2Carry out the high temperature sintering second time in the/Ar mixed atmosphere; H
2The ratio of/Ar mixed gas is 4-6%v/v, and flow is 16 ± 2ml/min; Sintering temperature is 1280 ± 10 ℃, and sintering time is 5 ± 1h, and behind the high temperature sintering, furnace temperature is lowered the temperature naturally;
Step 4: the sample behind the general's high temperature sintering second time grinds, compressing tablet, and milling time is 0.4h-1.5h, and pressure is 14-18Mpa during compressing tablet; Then at H
2Carry out high temperature sintering for the third time in the/Ar mixed atmosphere.H
2The ratio of/Ar mixed gas is 4-6%v/v, and flow is 10 ± 2ml/min; Sintering temperature is 1280 ± 10 ℃, and sintering time is 5 ± 1h, and behind the high temperature sintering, furnace temperature is lowered the temperature naturally;
The present invention fully prepares sample by atom in the raw material or ionic long-range diffusion theory.This preparation method comprises following preparation process: with pre-burning at high temperature behind the raw material thorough mixing of stoichiometric ratio, make carbonate decomposition, and initial reaction; The sample of pre-burning is carried out the high temperature sintering first time under the reducing atmosphere that flow is accurately controlled; Sample behind the first time high temperature sintering is ground compressing tablet, accurately carry out the high temperature sintering second time under the reducing atmosphere of control at flow; Sample behind the second time high temperature sintering is ground compressing tablet, and accurately carrying out for the third time under the reducing atmosphere of control at flow, high temperature burns.
The invention has the beneficial effects as follows: this incremental through the present invention, reject the sample that the method for dephasign is prepared step by step, not only purity is high, and the sample that magneto-resistance effect is prepared than traditional technology significantly improves.
Four, description of drawings
Fig. 1 is a preparation flow synoptic diagram of the present invention
Fig. 2 is the high-purity single-phase Sr that the present invention prepares
2FeMoO
6X ray diffracting spectrum
Fig. 3 is high-purity single-phase Sr
2FeMoO
6Theoretical X ray diffracting spectrum and experiment X ray diffracting spectrum contrast synoptic diagram, red line is theoretical X ray diffracting spectrum, the spectral line that annulus is linked to be is the X ray diffracting spectrum that the laboratory records, little vertical line is represented Prague peak position.
Fig. 4 is the high-purity single-phase Sr of the present invention
2FeMoO
6At 300K, the magneto-resistance effect synoptic diagram during 1.2T.
Five, embodiment
Embodiment: a) with the SrCO more than an amount of analytical pure
3(99.0%), Fe
2O
3(99.0%), MoO
3(99.5%) is placed on and carries out drying in the baking oven.
B) according to stoichiometric equation Sr
2FeMoO
6The mass ratio preparation SrCO of middle Sr, Fe, Mo
3(99.0%), Fe
2O
3(99.0%), MoO
3(99.5%) required composition, fully grinding mixes it.
C) with b) ground sample places the pre-burning of KSL-1700X high temperature sintering furnace, carbonate decomposed fully and initial reaction.
D) with c) sample of pre-burning fully grinds compressing tablet.
E) with d) sample behind the compressing tablet is at H
2Carry out the high temperature sintering first time in the/Ar mixed atmosphere.
F) with e) sample behind the first sintering fully grinds compressing tablet.
G) with f) sample behind the compressing tablet is at H
2Carry out the high temperature sintering second time in the/Ar mixed atmosphere.
H) with g) for the second time the sample behind the sintering fully grind compressing tablet.
I) with h) sample behind the compressing tablet is at H
2Carry out high temperature sintering for the third time in the/Ar mixed atmosphere.
Place the pre-burning of KSL-1700X high temperature sintering furnace, its technical characterictic is:
1) sintering temperature is 900 ℃, and sintering time is 10h.
2) after high temperature sintering finished, furnace temperature was lowered the temperature naturally.
The sample of pre-burning is fully ground, and compressing tablet, its technical characterictic are that milling time is 2.5-4h, and pressure is 14-18Mpa during compressing tablet.
At H
2Carry out the high temperature sintering first time in the/Ar mixed atmosphere,
1) H
2The ratio of/Ar mixed gas is 5%, and flow is 20ml/min.
2) sintering temperature is 1280 ℃.
3) sintering time is 5h.
4) behind the high temperature sintering, furnace temperature is lowered the temperature naturally.
With the sample behind the first time high temperature sintering grind, compressing tablet, milling time is 1.5-2h, pressure is 14-18Mpa during compressing tablet.
At H
2Carry out the high temperature sintering second time in the/Ar mixed atmosphere, its technical characterictic is:
1) H
2The ratio of/Ar mixed gas is 5%, and flow is 16ml/min.
2) sintering temperature is 1280 ℃.
3) sintering time is 5h.
4) behind the high temperature sintering, furnace temperature is lowered the temperature naturally.
With the sample behind the second time high temperature sintering grind, compressing tablet, milling time is 0.4h-1.5h, pressure is 14-18Mpa during compressing tablet.
At H
2Carry out high temperature sintering for the third time in the/Ar mixed atmosphere, its technical characterictic is:
1) H
2The ratio of/Ar mixed gas is 5%, and flow is 10ml/min.
2) sintering temperature is 1280 ℃.
3) sintering time is 5h.
4) behind the high temperature sintering, furnace temperature is lowered the temperature naturally.
Adopt planetary ball mill, its milling time is three times of above-mentioned milling time.
If adopt the underhand polish of agate jar, its milling time is 4h.Planetary ball mill then is 12h.
So far, the preparation of sample is accomplished, and is the quality of test sample, and we have done X-ray diffraction, and (X-ray diffraction XRD) analyzes, and its XRD figure spectrum is shown in accompanying drawing 2.The single phase property of XRD presentation of results sample is fine.In order to verify the quality of XRD figure spectrum, the XRD data have been carried out the Rietveld refine, its refine result is shown in accompanying drawing 3.For characterizing the magneto-resistance effect of this high-purity single-phase sample, it has been carried out the magneto-resistor measurement, the magneto-resistor measuring result of its 300K is shown in accompanying drawing four.Magneto-resistance effect 10% during with 300K, 7T is compared, and the sample of our preparation is at 300K, and the magneto-resistance effect during 1.2T has just reached 9%, and the intensity that this has just reduced magnetic field greatly makes this Pang magnetoresistance material see dawn in real-life application.
Claims (3)
1. high-purity single-phase Sr
2FeMoO
6The preparation method, it is characterized in that adopting following steps:
Step 1: with the SrCO more than the analytical pure
3(purity>=99.0wt%), Fe
2O
3(purity>=99.0wt%), MoO
3(purity>=99.5wt%) is placed on and carries out drying in the baking oven, then according to Sr
2FeMoO
6Stoichiometric equation prepare required composition, fully grind it mixed, place the high temperature sintering furnace pre-burning, sintering temperature is 900 ± 20 ℃, sintering time is 10 ± 1h; Initial reaction obtains sample to make carbonate decompose also fully;
Step 2: with the sample of pre-burning fully grind, compressing tablet, milling time is 2.5-4h, pressure is 14-18Mpa during compressing tablet; At H
2Carry out the high temperature sintering first time in the/Ar mixed atmosphere; H
2The ratio of/Ar mixed gas is 4-6%v/v, and flow is 20 ± 2ml/min; Sintering temperature is 1280 ± 10 ℃, and sintering time is 5 ± 1h, and behind the high temperature sintering, furnace temperature is lowered the temperature naturally;
Step 3: the sample behind the general's high temperature sintering first time grinds, compressing tablet, and milling time is 1.5-2h, and pressure is 14-18Mpa during compressing tablet; Then at H
2Carry out the high temperature sintering second time in the/Ar mixed atmosphere; H
2The ratio of/Ar mixed gas is 4-6%v/v, and flow is 16 ± 2ml/min; Sintering temperature is 1280 ± 10 ℃, and sintering time is 5 ± 1h, and behind the high temperature sintering, furnace temperature is lowered the temperature naturally;
Step 4: the sample behind the general's high temperature sintering second time grinds, compressing tablet, and milling time is 0.4h-1.5h, and pressure is 14-18Mpa during compressing tablet; Then at H
2Carry out high temperature sintering for the third time in the/Ar mixed atmosphere.H
2The ratio of/Ar mixed gas is 4-6%v/v, and flow is 10 ± 2ml/min; Sintering temperature is 1280 ± 10 ℃, and sintering time is 5 ± 1h, and behind the high temperature sintering, furnace temperature is lowered the temperature naturally.
2. high-purity single-phase Sr as claimed in claim 1
2FeMoO
6The preparation method, it is characterized in that carrying out in the baking oven drying, drying temperature is 200 ± 20 ℃, be 5 ± 1h time of drying.
3. high-purity single-phase Sr as claimed in claim 1
2FeMoO
6The preparation method, it is characterized in that fully grinding it is mixed, if adopt planetary ball mill, its milling time is three times of above-mentioned milling time.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633495A (en) * | 2012-04-11 | 2012-08-15 | 南京大学 | Preparation method of room-temperature ferromagnetic Sr2FemMonO6 ceramic |
| CN103193487A (en) * | 2013-04-22 | 2013-07-10 | 南京大学 | Method for quantitatively controlling B-position antiposition defect concentration of Sr2FeMoO6 ceramic |
| CN104961162A (en) * | 2015-06-30 | 2015-10-07 | 电子科技大学 | Preparation method of single pure-phase bismuth ferrite material based on ionic compensation |
| CN109046369A (en) * | 2018-09-25 | 2018-12-21 | 安徽大学 | A kind of photochemical catalyst Sr2FeMoO6Preparation method |
| CN113956027A (en) * | 2021-11-16 | 2022-01-21 | 武汉理工大学 | Ferrite wave-absorbing material and preparation method thereof |
Citations (1)
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| US7227773B1 (en) * | 2002-10-09 | 2007-06-05 | Grandis, Inc. | Magnetic element utilizing spin-transfer and half-metals and an MRAM device using the magnetic element |
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2011
- 2011-06-22 CN CN2011101689821A patent/CN102351524A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7227773B1 (en) * | 2002-10-09 | 2007-06-05 | Grandis, Inc. | Magnetic element utilizing spin-transfer and half-metals and an MRAM device using the magnetic element |
Non-Patent Citations (2)
| Title |
|---|
| 胡艳春等: "巨磁阻材料Sr1.9Gd0.1FeMoO6光掺杂的正电子湮没研究", 《信阳师范学院学报:自然科学版》 * |
| 路庆凤等: "钆掺杂巨磁阻材料Sr2FeMoO6正电子湮没谱", 《河南师范大学学报(自然科学版)》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633495A (en) * | 2012-04-11 | 2012-08-15 | 南京大学 | Preparation method of room-temperature ferromagnetic Sr2FemMonO6 ceramic |
| CN103193487A (en) * | 2013-04-22 | 2013-07-10 | 南京大学 | Method for quantitatively controlling B-position antiposition defect concentration of Sr2FeMoO6 ceramic |
| CN104961162A (en) * | 2015-06-30 | 2015-10-07 | 电子科技大学 | Preparation method of single pure-phase bismuth ferrite material based on ionic compensation |
| CN104961162B (en) * | 2015-06-30 | 2017-03-08 | 电子科技大学 | A kind of method that single pure phase bismuth ferric material is prepared based on Lithium ions compensation |
| CN109046369A (en) * | 2018-09-25 | 2018-12-21 | 安徽大学 | A kind of photochemical catalyst Sr2FeMoO6Preparation method |
| CN113956027A (en) * | 2021-11-16 | 2022-01-21 | 武汉理工大学 | Ferrite wave-absorbing material and preparation method thereof |
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Application publication date: 20120215 |