CN104072123A - Perovskite YCoxFe(1-x)O3 oxide crystal and preparation method thereof - Google Patents

Perovskite YCoxFe(1-x)O3 oxide crystal and preparation method thereof Download PDF

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CN104072123A
CN104072123A CN201410263899.6A CN201410263899A CN104072123A CN 104072123 A CN104072123 A CN 104072123A CN 201410263899 A CN201410263899 A CN 201410263899A CN 104072123 A CN104072123 A CN 104072123A
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crystal
preparation
yco
powder
perovskite oxide
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谢文辉
李晓红
魏莹芬
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East China Normal University
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Abstract

The invention discloses a perovskite oxide crystal and a preparation process thereof. The crystal is an orthogonal perovskite crystal with a chemical formula YCoXFe(1-x)O3, wherein 0.1<=x<=0.9; the space group of the crystal is Pnma, and character constants are shown in the specification. In the invention, with Y(NO3)3.6H2O, Co(NO3)2.6H2O and Fe(NO3)3.6H2O as raw materials, a precursor of Y2CoxFe(1-x)O6 is prepared by a sol-gel process and subjected to drying, pyrolysis, grinding and presintering, and finally, the perovskite oxide YCoxFe(1-x)O3 crystal is synthesized at a high temperature of 1,050-1,100 DEG C. The YCoxFe(1-x)O3 crystal disclosed by the invention provides a broad application prospect for systematic research of the properties of series of compounds, fuel cells, catalytic electrodes and sensors.

Description

Uhligite YCo xfe 1-xo 3oxide crystal and preparation method thereof
Technical field
The present invention relates to a kind of perovskite oxide YCo xfe 1-Xo 3crystal and preparation method thereof and at electrode materials, the application in sensor and photocatalysis field etc.
Background technology
Since 1950S, for uhligite ABO 3the structure of oxide compound and performance just have a lot of research.Researchist finds to exist in uhligite system the performance that a series of using values are very high, high-temperature superconductor for example, room temperature giant magnetoresistance effect, room temperature tunnelling type giant magnetoresistance effect, photocatalysis performance etc.Due to its special catalytic, magnetic, dielectricity and huge magnetic impedance character, thereby make the compound of this system receive concern highly.The YFeO of perovskite structure 3, YCoO 3crystalline material all has important using value in electrode materials, sensor and photocatalysis field.In the preparation of conventional high-temperature solid reaction process, because its deficiency has a lot, for example sintering temperature is too high, needs repeated multiple times sintering, easily produces dephasign etc., and these all can affect the performance of product to a great extent.
Summary of the invention
The object of the present invention is to provide a kind of perovskite oxide YCo xfe 1-Xo 3crystal, another object of the present invention is to provide the method for preparing this compound.For overcoming existing preparation method's above-mentioned deficiency, the present invention proposes to adopt sol-gel method to prepare precursor first, and high temperature sintering synthesizes uhligite YCo xfe 1-Xo 3the preparation method of (0.1≤x≤0.9) oxide crystal.
The present invention has proposed a kind of perovskite oxide crystal first, and the chemical formula of this crystal is YCo xfe 1-Xo 3, 0.1≤x≤0.9; This YCo xfe 1-Xo 3crystal is quadrature perovskite crystal, and spacer is Pnma, character constant
The invention allows for a kind of new perovskite oxide crystal YCo xfe 1-Xo 3the preparation method of (0.1≤x≤0.9), with Y (NO 3) 36H 2o, Co (NO 3) 26H 2o, Fe (NO 3) 36H 2o is raw material, utilizes sol-gel method to prepare Y 2co xfe 1-Xo 6presoma, drying, pyrolysis, grinding, pre-burning, at 1050 ℃-1100 ℃, high temperature is synthetic, prepares described perovskite oxide crystal YCo xfe 1-Xo 3, 0.1≤x≤0.9.
Preparation method of the present invention, concrete steps comprise following:
A. according to 1: x: mol ratio (1-x) takes respectively analytically pure Y (NO 3) 36H 2o, Co (NO 3) 26H 2o, Fe (NO 3) 36H 2o, 0.1≤x≤0.9, adds appropriate deionized water dissolving, obtains nitrate solution;
According to n (metal ion): n (citric acid)=within 1: 1.5, mol ratio takes analytically pure citric acid C 6h 8o 7h 2o, is dissolved in deionized water, obtains citric acid solution.
B. the above-mentioned citric acid solution preparing is dropwise added in aforementioned nitrate solution, then add appropriate ethylene glycol, the pH value of solution is adjusted to 5-7, and stirs 3-6 hour.Preferably, use the pH value to 6 of ammoniacal liquor regulator solution.Preferably, stir 5 hours.
C. above-mentioned solution is put into the water-bath of 80 ℃, constant temperature stirs, and to solvent evaporates, forms clear gel, gained solid after described clear gel is dry, then grind into powder.Preferably, described clear gel is placed in baking oven, at 160 ℃ dry 24 hours.Preferably, described in the powder that grinds to form be placed in 80 ℃ of oven dry of loft drier, the powder of oven dry is crossed to 120 mesh sieves.
D. powder step c being made is put into alumina crucible, first with 900 ℃ of presintering, cooling after, powder is ground again and briquetting carries out sintering for the second time, according to the difference of X value, sintering temperature is at 1050-1100 ℃.
In described steps d, powder is put into after alumina crucible, drips massfraction and be the polyvinyl alcohol solution of 4-8% as tackiness agent in described powder; The add-on of described polyvinyl alcohol solution is the 3-6% of described powder quality.Preferably, in described powder, dripping massfraction is that 6% polyvinyl alcohol solution is as tackiness agent; The add-on of described polyvinyl alcohol solution is 5% of described powder quality.
In described steps d, the pre-burning time of presintering is 5-8 hour.Preferably, the pre-burning time is 7 hours.
In described steps d, the sintering time of sintering is 8-12 hour for the second time.Preferably, the sintering time of sintering is 10 hours for the second time.
In described steps d, described briquetting carries out under 30-50MPa pressure.Preferably, described briquetting carries out under 40MPa pressure.
In described steps d, put into before alumina crucible sintering, in alumina crucible, be added with bedding and padding, carry out sintering for the second time.Temperature rise rate with 2 ℃/min keeps 2h plastic removal at 500 ℃, and then according to the difference of x value, sintering temperature is at 1050-1100 ℃, and sintering time is 10 hours.Temperature-fall period is set 2 ℃/min programmed cooling to room temperature.
Through above step, make perovskite oxide crystal YCo of the present invention xfe 1-Xo 3.
The present invention successfully synthesizes YCo first xfe 1-Xo 3crystal.Preparation method of the present invention is easy to implement, and sintering temperature is low, and finished product purity is high, the product YCo of gained xfe 1-Xo 3crystal belongs to weak ferromagnetism, and it has the wide application prospect of character, fuel cell, catalysis electrode and the sensor each side of systematic study series compound.
Accompanying drawing explanation
Fig. 1 is perovskite oxide crystal YCo of the present invention xfe 1-Xo 3the structural representation of crystal.
Fig. 2 is perovskite oxide crystal YCo of the present invention xfe 1-Xo 3the X ray diffracting spectrum (XRD) of crystal (x=0.5).
Fig. 3 is perovskite oxide crystal YCo of the present invention xfe 1-Xo 3the magnetic moment of crystal (x=0.5) under 100oe magnetic field and the relation curve of temperature.
Embodiment
In conjunction with following specific embodiments and the drawings, the present invention is described in further detail, and protection content of the present invention is not limited to following examples.Do not deviating under the spirit and scope of inventive concept, variation and advantage that those skilled in the art can expect are all included in the present invention, and take appending claims as protection domain.Implement process of the present invention, condition, reagent, experimental technique etc., except the content of mentioning specially below, be universal knowledege and the common practise of this area, the present invention is not particularly limited content.
A kind of perovskite oxide YCo of the present invention xfe 1-Xo 3crystal, this crystal is quadrature perovskite crystal, spacer is Pnma, character constant 0.1≤X≤0.9 wherein.
The invention provides perovskite oxide YCo xfe 1-Xo 3the preparation method of crystal, is specially:
A. according to 1: x: mol ratio (1-x) takes respectively analytically pure Y (NO 3) 36H 2o, Co (NO 3) 26H 2o, Fe (NO 3) 36H 2o, adds appropriate deionized water dissolving.According to n (metal ion): n (citric acid)=within 1: 1.5, mol ratio takes analytically pure citric acid C 6h 8o 7h 2o, is dissolved in deionized water.
B. the citric acid solution preparing is dropwise added in nitrate solution, then add appropriate ethylene glycol, with ammoniacal liquor, the pH value of solution is adjusted to 5-7, and stir 5 hours.
C. solution is put into the water-bath of 80 ℃, constant temperature stirs and to make to form transparent gel after solvent evaporates, afterwards by gel in baking oven in 160 ℃ dry 24 hours, by the solid grinding powder of gained.
D. powder step c being made is put into alumina crucible, and first with 900 ℃ of presintering, the pre-burning time is 8 hours, after cooling, powder is ground again to also briquetting and carry out sintering for the second time, according to the difference of X value, sintering temperature is at 1050-1100 ℃, and sintering time is 10 hours.
Described steps d drips massfraction and is 6% polyvinyl alcohol solution as tackiness agent in powder, and the add-on of polyvinyl alcohol solution is powder quality 5%, puts into 80 ℃ of oven dry of loft drier after grinding, and the powder of oven dry is crossed to 120 mesh sieves.Gained powder is pressed into bulk under 40MPa pressure, puts into before alumina crucible sintering, in alumina crucible, be added with bedding and padding, carry out sintering for the second time.Temperature rise rate with 2 ℃/min keeps 2h plastic removal at 500 ℃, and then according to the difference of X value, sintering temperature is at 1050-1100 ℃, and sintering time is 10 hours.Temperature-fall period is set 2 ℃/min programmed cooling to room temperature, makes finished product.
Embodiment 1: perovskite oxide YCo xfe 1-Xo 3(x=0.1) preparation of crystal
A. by the mol ratio of 1: 0.1: 0.9, take respectively analytically pure 1.915g Y (NO 3) 36H 2o, 0.146gCo (NO 3) 26H 2o, 1.818g Fe (NO 3) 36H 2o, x=0.1, adds appropriate deionized water dissolving.According to n (metal ion): n (citric acid)=within 1: 1.5, mol ratio takes analytically pure 3.152g citric acid C 6h 8o 7h 2o, is dissolved in the deionized water of 20ml.
B. the citric acid solution preparing is dropwise added in nitrate solution, then add the ethylene glycol of 10ml, with ammoniacal liquor, the pH value of solution is adjusted to 5-7, and stir 5 hours.
C. solution is put into the water-bath of 80 ℃, constant temperature stirs and to make to form transparent gel after solvent evaporates, afterwards by gel in baking oven in 160 ℃ dry 24 hours, by the solid grinding powder of gained.
D. powder step c being made is put into alumina crucible, and first with 900 ℃ of presintering, the pre-burning time is 8 hours, powder is ground again after cooling and briquetting carries out sintering for the second time, and sintering temperature is at 1100 ℃, and sintering time is 10 hours.
Described steps d drips massfraction and is 6% polyvinyl alcohol solution as tackiness agent in powder, and the add-on of polyvinyl alcohol solution is powder quality 5%, puts into 80 ℃ of oven dry of loft drier after grinding, and the powder of oven dry is crossed to 120 mesh sieves.Gained powder is pressed into bulk under 40MPa pressure, puts into before alumina crucible sintering, in alumina crucible, be added with bedding and padding, carry out sintering for the second time.Temperature rise rate with 2 ℃/min keeps 2h plastic removal at 500 ℃, and sintering temperature is at 1100 ℃, and sintering time is 10 hours.Temperature-fall period is set 2 ℃/min programmed cooling to room temperature, makes finished product perovskite oxide crystal YCo xfe 1-Xo 3(x=0.1), its structure as shown in Figure 1, is typical quadrature perovskite structure, and spacer is Pnma, and character constant is
Embodiment 2: perovskite oxide YCo xfe 1-Xo 3(x=0.2) preparation technology of crystal.
By the mol ratio of 1: 0.2: 0.8, take respectively analytically pure 1.915g Y (NO 3) 36H 2o, 0.291g Co (NO 3) 26H 2o, 1.616g Fe (NO 3) 36H 2o, according to n (metal ion): n (citric acid)=within 1: 1.5, mol ratio takes analytically pure 3.152g citric acid C 6h 8o 7h 2o, other step is with embodiment 1.The perovskite oxide crystal YCo preparing xfe 1-Xo 3(x=0.2), its structure as shown in Figure 1, is typical quadrature perovskite structure, and spacer is Pnma, and character constant is
Embodiment 3: perovskite oxide YCo xfe 1-Xo 3(x=0.3) preparation technology of crystal.
By the mol ratio of 1: 0.3: 0.7, take respectively analytically pure 1.915g Y (NO 3) 36H 2o, 0.437g Co (NO 3) 26H 2o, 1.414g Fe (NO 3) 36H 2o, according to n (metal ion): n (citric acid)=within 1: 1.5, mol ratio takes analytically pure 3.152g citric acid C 6h 8o 7h 2o, other step is with embodiment 1.The perovskite oxide crystal YCo preparing xfe 1-Xo 3(x=0.3), its structure as shown in Figure 1, is typical quadrature perovskite structure, and spacer is Pnma, and character constant is
Embodiment 4: perovskite oxide YCo xfe 1-Xo 3(x=0.4) preparation technology of crystal.
By the mol ratio of 1: 0.4: 0.6, take respectively analytically pure 1.915g Y (NO 3) 36H 2o, 0.582g Co (NO 3) 26H 2o, 1.212g Fe (NO 3) 36H 2o, according to n (metal ion): n (citric acid)=within 1: 1.5, mol ratio takes analytically pure 3.152g citric acid C 6h 8o 7h 2o, other step is with embodiment 1.The perovskite oxide crystal YCo preparing xfe 1-Xo 3(x=0.4), its structure as shown in Figure 1, is typical quadrature perovskite structure, and spacer is Pnma, and character constant is
Embodiment 5: perovskite oxide YCo xfe 1-Xo 3(x=0.5) preparation technology of crystal.
By the mol ratio of 1: 0.5: 0.5, take respectively analytically pure 1.915g Y (NO 3) 36H 2o, 0.728g Co (NO 3) 26H 2o, 1.01gFe (NO 3) 36H 2o, according to n (metal ion): n (citric acid)=within 1: 1.5, mol ratio takes analytically pure 3.152g citric acid C 6h 8o 7h 2o, other step is with embodiment 1, the product perovskite oxide product body YCo obtaining xfe 1-Xo 3(x=0.5), its structure as shown in Figure 1, is typical quadrature perovskite structure, and as shown in Figure 2, from diffracting spectrum, the spacer of this crystal is Pnma to its X ray diffracting spectrum (XRD).Character constant is the product perovskite oxide crystal YCo obtaining xfe 1-Xo 3(x=0.5) relation curve of the magnetic moment under 100oe magnetic field and temperature, as shown in Figure 3, Fig. 3 is visible, and this crystalline material has weak ferromagnetism.
Embodiment 6: perovskite oxide YCo xfe 1-Xo 3(x=0.6) preparation technology of crystal.
By the mol ratio of 1: 0.6: 0.4, take respectively analytically pure 1.915g Y (NO 3) 36H 2o, 0.873g Co (NO 3) 26H 2o, 0.808g Fe (NO 3) 36H 2o, according to n (metal ion): n (citric acid)=within 1: 1.5, mol ratio takes analytically pure 3.152g citric acid C 6h 8o 7h 2o, at 1050 ℃ of sintering 10h, other step is with embodiment 1.The perovskite oxide crystal YCo obtaining xfe 1-Xo 3(x=0.6), its structure as shown in Figure 1, is typical quadrature perovskite structure, and spacer is Pnma, and character constant is
Embodiment 7: perovskite oxide YCo xfe 1-Xo 3(x=0.7) preparation technology of crystal.
By the mol ratio of 1: 0.7: 0.3, take respectively analytically pure 1.915g Y (NO 3) 36H 2o, 1.019g Co (NO 3) 26H 2o, 0.606g Fe (NO 3) 36H 2o, according to n (metal ion): n (citric acid)=within 1: 1.5, mol ratio takes analytically pure 3.152g citric acid C 6h 8o 7h 2o, at 1050 ℃ of sintering 10h, other step is with embodiment 1.The perovskite oxide crystal YCo obtaining xfe 1-Xo 3(x=0.7), its structure as shown in Figure 1, is typical quadrature perovskite structure, and spacer is Pnma, and character constant is
Embodiment 8: perovskite oxide YCo xfe 1-Xo 3(x=0.8) preparation technology of crystal.
By the mol ratio of 1: 0.8: 0.2, take respectively analytically pure 1.915g Y (NO 3) 36H 2o, 1.164g Co (NO 3) 26H 2o, 0.404g Fe (NO 3) 36H 2o, according to n (metal ion): n (citric acid)=within 1: 1.5, mol ratio takes analytically pure 3.152g citric acid C 6h 8o 7h 2o, at 1050 ℃ of sintering 10h, other step is with embodiment 1, and the product obtaining is typical quadrature perovskite structure, and spacer is Pnma, and character constant is
Embodiment 9: perovskite oxide YCo xfe 1-Xo 3(x=0.9) preparation technology of crystal.
By the mol ratio of 1: 0.9: 0.1, take respectively analytically pure 1.915g Y (NO 3) 36H 2o, 1.31gCo (NO 3) 26H 2o, 0.202g Fe (NO 3) 36H 2o, according to n (metal ion): n (citric acid)=within 1: 1.5, mol ratio takes analytically pure 3.152g citric acid C 6h 8o 7h 2o, at 1050 ℃ of sintering 10h, other step is with embodiment 1.The product obtaining is perovskite oxide crystal YCo xfe 1-Xo 3(x=0.9), its structure as shown in Figure 1, is typical quadrature perovskite structure, and spacer is Pnma, and lattice parameter is

Claims (10)

1. a perovskite oxide crystal, is characterized in that, described crystal is quadrature perovskite crystal, and its chemical formula is: YCo xfe 1-Xo 3, 0.1≤x≤0.9; Described crystal space group is Pnma, character constant
2. a preparation method for perovskite oxide crystal, is characterized in that, with Y (NO 3) 36H 2o, Co (NO 3) 26H 2o, Fe (NO 3) 36H 2o is raw material, utilizes sol-gel method to make Y 2co xfe 1-Xo 6presoma, then drying, pyrolysis, grinding, pre-burning, at 1050 ℃-1100 ℃, high temperature is synthetic, prepares perovskite oxide crystal YCo as claimed in claim 1 xfe 1-Xo 3, 0.1≤x≤0.9.
3. preparation method as claimed in claim 2, is characterized in that, concrete steps are as follows:
A. according to 1: x: mol ratio (1-x) takes respectively analytically pure Y (NO 3) 36H 2o, Co (NO 3) 26H 2o, Fe (NO 3) 36H 2o, 0.1≤x≤0.9, adds deionized water dissolving, obtains nitrate solution; According to n (metal ion): n (citric acid)=within 1: 1.5, mol ratio takes analytically pure citric acid C 6h 8o 7h 2o, is dissolved in deionized water, obtains citric acid solution;
B. described citric acid solution is dropwise added in described nitrate solution, add ethylene glycol, regulate pH value to 5-7;
C. above-mentioned solution constant temperature at 80 ℃ is stirred, form clear gel after solvent evaporates, dry described clear gel, by the solid abrasive powdered of gained;
D. powder step c being made is put into alumina crucible, first with 900 ℃ of presintering, powder is ground again after cooling and briquetting carries out sintering for the second time, and sintering temperature is 1050-1100 ℃ for the second time; Prepare described perovskite oxide crystal YCo xfe 1-Xo 3, 0.1≤x≤0.9.
4. preparation method as claimed in claim 3, is characterized in that, in described step b, with ammoniacal liquor, regulates pH value.
5. preparation method as claimed in claim 3, is characterized in that, in described step c, described in the powder that grinds to form be placed in 80 ℃ of oven dry of loft drier, cross 120 mesh sieves.
6. preparation method as claimed in claim 3, is characterized in that, in described steps d, drips massfraction and be 6% polyvinyl alcohol solution as tackiness agent in described powder; The add-on of described polyvinyl alcohol solution is 5% of described powder quality.
7. preparation method as claimed in claim 3, is characterized in that, in described steps d, described briquetting carries out under 30-50MPa pressure.
8. preparation method as claimed in claim 3, is characterized in that, in described steps d, with the temperature rise rate of 2 ℃/min, at 500 ℃, keeps 2h plastic removals; Rate of temperature fall with 2 ℃/min is cooled to room temperature.
9. preparation method as claimed in claim 3, is characterized in that, in described steps d, the pre-burning time of presintering is 5-8 hour.
10. preparation method as claimed in claim 3, is characterized in that, in described steps d, the time of sintering is 8-12 hour for the second time.
CN201410263899.6A 2014-06-13 2014-06-13 Perovskite YCoxFe(1-x)O3 oxide crystal and preparation method thereof Pending CN104072123A (en)

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CN113185267A (en) * 2021-05-28 2021-07-30 郑州轻工业大学 Cobalt-doped perovskite ceramic and preparation method thereof
CN114988482A (en) * 2022-07-11 2022-09-02 中汽创智科技有限公司 Perovskite type solid electrolyte and preparation method and application thereof

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CN109046379A (en) * 2018-06-29 2018-12-21 华东师范大学 A kind of perovskite composite oxides load platinum catalyst and its preparation and application
CN113185267A (en) * 2021-05-28 2021-07-30 郑州轻工业大学 Cobalt-doped perovskite ceramic and preparation method thereof
CN113185267B (en) * 2021-05-28 2022-12-20 郑州轻工业大学 Cobalt-doped perovskite ceramic and preparation method thereof
CN114988482A (en) * 2022-07-11 2022-09-02 中汽创智科技有限公司 Perovskite type solid electrolyte and preparation method and application thereof

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Application publication date: 20141001