CN104876275A - Low temperature preparation method of layered perovskite - Google Patents
Low temperature preparation method of layered perovskite Download PDFInfo
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Abstract
The invention discloses a low temperature preparation method of Ruddlesden-Popper type layered perovskite. By using ''chloride ion induction effect'', a uniform layered precursor containing the chloride ions is formed, then the chloride ions in the precursor are dissociated and removed, and thus the layered structure is obtained. Compared with a traditional R-P type layered perovskite preparation method, the method has the advantage that the preparation temperature in the method is greatly reduced, so that the application scope of the type of the materials is expanded. The obtained materials possess high performance in the aspects of specific surface, thermal stability, electromagnetic performance, catalytic activity and the like.
Description
Technical field
The present invention relates to a kind of preparation method of laminated perovskite, particularly relate to a kind of Ruddlesden-Popper type laminated perovskite A
3b
2o
7low temperature preparation method.
Background technology
Ruddlesden-Popper(R-P) type laminated perovskite is a kind of perovskite-like type composite oxides with laminate structure, and its molecular formula can be abbreviated as A
n+1b
no
3n+1or AO (ABO
3) n, its basic structure can think that halite layer AO inserts original uhligite and the two-dimentional intercalation configuration formed.Sequential 2 D makes it have superior thermostability; Meanwhile, the halite layer AO comprising macrocation defines loose specular layer, is conducive to the interlayer transmission of oxygenate kind or ion, makes it have superior transmission performance.From nineteen fifty-seven, S. N. Ruddlesden and P. Popper has synthesized Sr first
3ti
2o
7(S. N. Ruddlesden and P. Popper, Acta Cryst., 1958,11,54.) since, superior oxygen transmission performance, thermodynamic stability and thermochemistry consistency make such material earn widespread respect, and have good Research Prospects in fields such as electricity, magnetic, light, catalysis, oxygen permeable film, intermediate temperature fuel cells.Y. Maeno etc. (Y. Maeno et al., Nature, 1994,372,532-534.) report R-P type laminated perovskite Sr
2ruO
4supraconductivity, even if find that laminated perovskite still has superior conductivity not containing Cu element.K.-N. Jung etc. (K.-N. Jung et al., Chem. Commun., 2012,48,9406-9408.) find at Li-O
2in battery, laminated perovskite La
1.7ca
0.3ni
0.75cu
0.25o
4significantly can promote Li
2o
2oxidation.Be widely studied in magnetic fields as ferromagnetic laminated perovskite.Y. Moritomo etc. (Y. Moritomo et al., Nature, 1996,380,141-144.) report laminated perovskite (La, Sr)
n+1mn
no
3n+1giant magnetoresistance effect.H. Asano etc. (H. Asano et al., Appl. Phys. Lett., 1997,70,2303-2305.) have studied laminated perovskite La afterwards
2-2xca
1+2xmn
2o
7in epitaxial film and polycrystalline bulk time magnetic transport performance.D. Neiner etc. (D. Neiner et al., Chem. Mater., 2006,
18, 518-524.) and synthesize laminated perovskite Li
0.3ni
0.85la
2ti
3o
10, this compound presents ferromegnetism rarely found in nickel-based oxide.In addition, the ionic channel that laminated perovskite is loose makes it come into one's own gradually in photocatalysis field.Reported have Pb
2ga
2nb
2o
10and RbPb
2nb
2o
7(K.G. Kanade et al., Int. J. Hydrogen Energ., 2008,33,6904-6912.), ABi
2ta
2o
9(A=Ca, Sr, Ba) (Y. Li et al., J. Solid State Chem., 2008,181,2653-2659.) etc.But, laminated perovskite high-performance further expand and study the restriction being but subject to its preparation condition.Traditional technology of preparing condition is harsh, generally needs high temperature (>=1300 ° of C), high pressure and longer calcination time (15 ~ 36 h) (N.H. Hur et al., Solid State Commun., 1999,112,61-65; T. Murata et al., J. Magn. Magn. Mater., 2006,303,138-141; Y. Tsujimoto et al., Chem. Commun., 2011,47,3263-3265.).This causes such material generally to have lower specific surface area, and preparation condition harshness causes implementing difficulty, is unfavorable for its widespread use.
Summary of the invention
The object of the invention is to obtain a kind of simple to operate, suitability wide and prepare Ruddlesden-Popper(R-P at a lower temperature) method of type laminated perovskite.
The object of the invention is to be achieved through the following technical solutions:
The present invention is the method for a kind of low-temperature growth R-P type laminated perovskite proposed on the basis of sol-gel method, we utilize " chlorion inductive effect " to form the stratiform presoma containing chlorion, detach the chlorion in removing precursor again, thus obtain laminate structure.
A low temperature preparation method for laminated perovskite, it is characterized in that the method successively step be:
1) by La
3+, Ce
3+, Sr
2+, Ca
2+, Ba
2+one or more salt and Mn
2+, Co
2+, Ni
2+, Zr
4+, Ti
4+one or more salt mix water-soluble formation solution A, by the chlorine source containing chlorion and the common water-soluble formation solution B of coordination agent, described coordination agent is one or more of PVA after citric acid, EDTA, glycine, degraded and citric acid glycol ester; Mixing A and B solution, stir, dehydration, dry, the precursor powder of calcining acquisition containing chlorion;
2) in a kettle., under alkaline condition, hydro-thermal or solvent heat treatment are carried out to precursor powder, after filtration, washing, drying, calcining, obtain target product and Ruddlesden-Popper type laminated perovskite.
In the present invention, the chlorine-containing compound as chlorine source is one or more of the hydrochloride of metal, p-Chlorobenzoic acid amide and ammonium chloride.
In the present invention, the calcining temperature of precursor is 600 ° of C ~ 1100 ° C.
In the present invention, basic solution precursor being carried out to hydro-thermal or solvent heat treatment is NH
4hCO
3, (NH
4)
2cO
3, NH
3h
2o, K
2cO
3, methane amide, trolamine, pyridine, aniline, quadrol, one or more water formed of anionite-exchange resin, ethanol or ethylene glycol solutions.
In the present invention, the temperature of precursor being carried out to hydrothermal treatment consists or solvent heat treatment is 80 ° of C ~ 220 ° C.
In the present invention, the calcining temperature of final product is 600 ° of C ~ 1100 ° C.
Outstanding feature of the present invention is:
Compared with traditional R-P type laminated perovskite preparation method, preparation temperature reduces greatly, and the range of application of such material is expanded; Simple to operate, expense is cheap, can adapt to the needs of large-scale commercial production; Resulting materials shows high-performance in specific surface, thermostability, electromagnetic performance, catalytic activity etc.; " chlorion inductive effect " thought in the method extends in the synthesis of nanometer complex oxide material.
Accompanying drawing explanation
Fig. 1 is product La
3mn
2o
7+ δpowder x-ray diffraction spectrogram.
Fig. 2 is product LaCa
2mn
2o
7powder x-ray diffraction spectrogram.
Embodiment
There is provided following examples for setting forth spy of the present invention further, but embodiments of the present invention are not limited to following examples.
Embodiment 1:
By 6.50 g La (NO
3)
36H
2o (15 mmol), 2.68 g Mn (NO
3)
2solution (50 wt%, 7.5 mmol), and 0.50 g MnCl
2(2.5 mmol) is water-soluble, forms solution A; By 6.33 g citric acids (30 mmol) and 2.25 g NH
4hCO
3(28.5 mmol) is water-soluble, forms solution B.Mixed with B solution by A, stir, underpressure distillation, dehydration forms denseer jelly, and drying afterwards, roasting 5 h under 700 ° of C, obtain blue-black precursor powder.Take 1.00 g precursor powder, contain 0.10 mol L
-1nH
4hCO
3in the autoclave of solution, react 12 h under 80 ° of C, suction filtration is separated, deionized water, washing with alcohol, and dry, roasting 2 h under 800 ° of C, obtains blue-black laminated perovskite La thereupon
3mn
2o
7+ δpowder.
Embodiment 2:
By 2.17 g La (NO
3)
36H
2o (5 mmol), 2.39 g Ca (NO
3)
24H
2o (10 mmol), 2.68 g Mn (NO
3)
2solution (50 wt%, 7.5 mmol), and 0.50 g MnCl
2(2.5 mmol) is water-soluble, forms solution A; By 6.33 g citric acids (30 mmol) and 2.25 g NH
4hCO
3(28.5 mmol) is water-soluble, forms solution B.Mixed with B solution by A, stir, underpressure distillation, dehydration forms denseer jelly, and dry, roasting 5 h under 800 ° of C, obtains precursor powder thereupon.Take 1.00 g precursor powder, contain 0.10 mol L
-1nH
4hCO
3in the autoclave of solution, react 12 h under 120 ° of C, suction filtration is separated, deionized water, washing with alcohol, and dry, roasting 2 h under 800 ° of C, obtains laminated perovskite LaCa thereupon
2mn
2o
7powder.
Embodiment 3:
By 1.73 g La (NO
3)
36H
2o (4 mmol), 0.53 g Ba (NO
3)
2and 1.17 g Co (NO
3)
26H
2o (4 mmol) is water-soluble, forms solution A; By water-soluble to 2.53 g citric acids (12 mmol) and 0.26 g p-Chlorobenzoic acid amide (2 mmol), form solution B.Mixed with B solution by A, stir, underpressure distillation, dehydration forms denseer jelly, and dry, roasting 2 h under 1000 ° of C, obtains precursor powder thereupon.Take 1.00 g precursor powder, contain 0.10 mol L
-1nH
4hCO
3in the autoclave of solution, react 8 h under 120 ° of C, rear suction filtration is separated, deionized water, washing with alcohol, and dry, roasting 2 h under 700 ° of C, obtains blue-black laminated perovskite La thereupon
2baCo
2o
7powder.
Embodiment 4:
By 1.30 g La (NO
3)
36H
2o (3 mmol), 1.27 g Sr (NO
3)
24H
2o (6 mmol), and 2.15 g Mn (NO
3)
2solution (50 wt%, 6 mmol) is water-soluble, forms solution A; By water-soluble to 3.80 g citric acids (18 mmol) and 0.38 g p-Chlorobenzoic acid amide (3 mmol), form solution B.Mixed with B solution by A, stir, underpressure distillation, dehydration forms denseer jelly, and dry, roasting 5 h under 700 ° of C, obtains precursor powder thereupon.Take 1.00 g precursor powder, in the autoclave containing the methane amide aqueous solution, react 6 h under 150 ° of C, suction filtration is separated, deionized water, washing with alcohol, and dry, roasting 2 h under 700 ° of C, obtains laminated perovskite LaSr thereupon
2mn
2o
7powder.
Embodiment 5:
By 1.43 g Ca (NO
3)
24H
2o (6 mmol), 1.29 g Zr (NO
3)
45H
2o (3 mmol), and 0.33 g ZrOCl
28H
2o (1 mmol) is water-soluble, forms solution A; By 2.53 g citric acids (12 mmol) and 0.79 g NH
4hCO
3(10 mmol) is water-soluble, forms solution B.Mixed with B solution by A, stir, underpressure distillation, dehydration forms denseer jelly, and dry, roasting 5 h under 800 ° of C, obtains precursor powder thereupon.Take 1.00 g precursor powder, containing in the autoclave of formamide soln, react 8 h under 160 ° of C, suction filtration is separated, deionized water, washing with alcohol, and dry, roasting 2 h under 800 ° of C, obtains laminated perovskite Ca thereupon
3zr
2o
7powder.
Embodiment 6:
By 0.87 g La (NO
3)
36H
2o (2 mmol), 0.95 g Ca (NO
3)
24H
2o (4 mmol), 1.29 g Zr (NO
3)
45H
2o (3 mmol), and 0.33 g ZrOCl
28H
2o (1 mmol) is water-soluble, forms solution A; 2.53 g citric acids are mixed with 1.12 g ethylene glycol, after esterification, obtains citric acid glycol ester, be dissolved in distilled water, obtain solution B.Mixing A and B solution, stir, underpressure distillation, and dehydration forms denseer jelly, and dry, roasting 5 h under 700 ° of C, obtains precursor powder thereupon.Taking 1.00 g precursor powder, is reaction medium with ethylene glycol, adds 3.00 g 717 type anionite-exchange resin, in autoclave, react 6 h under 200 ° of C, suction filtration is separated, deionized water, washing with alcohol, drying, roasting 2 h under 800 ° of C, obtains laminated perovskite LaCa thereupon
2zr
2o
7powder.
Embodiment 7:
By 0.87 g Ce (NO
3)
36H
2o (2 mmol), 1.05 g Ba (NO
3)
2(4 mmol), 1.07 g Mn (NO
3)
2solution (50 wt%, 3 mmol), and 0.20 g MnCl
2(1 mmol) is water-soluble, forms solution A; 2.53 g citric acids are mixed with 1.12 g ethylene glycol, after esterification, obtains citric acid glycol ester, be dissolved in distilled water, obtain solution B.Mixing A and B solution, underpressure distillation, dehydration forms denseer jelly, and dry, roasting 5 h under 800 ° of C, obtains precursor powder thereupon.Take 1.00 g precursor powder, with the mixing solutions (1: 2) of water and ethylene glycol for medium, add 1.06 g aniline, in autoclave, react 5 h under 180 ° of C, suction filtration is separated, deionized water, washing with alcohol, drying, roasting 2 h under 700 ° of C, obtains laminated perovskite CeBa thereupon
2mn
2o
7powder.
Embodiment 8:
By 2.60 g La (NO
3)
36H
2o (6 mmol), 1.07 g Mn (NO
3)
2solution (50 wt%, 3 mmol), and 0.20 g MnCl
2(1 mmol) is water-soluble, forms solution A; 4.40 g polyvinyl alcohol (PVA) are dissolved in distilled water, are made into the aqueous solution of 7%, after degraded, are solution B.Mixed with B solution by A, stir, underpressure distillation, dehydration forms denseer jelly, and dry, roasting 2 h under 750 ° of C, obtains precursor powder thereupon.Take 1.00 g precursor powder, in the autoclave containing the trolamine aqueous solution, react 5 h under 180 ° of C, suction filtration is separated, deionized water, washing with alcohol, and dry, roasting 2 h under 700 ° of C, obtains blue-black laminated perovskite La thereupon
3mn
2o
7+ δpowder.
Embodiment 9:
1.36 g tetrabutyl titanates (4 mmol) are dissolved in ethanol, add 1.43 g Ca (NO
3)
24H
2o (6 mmol), slowly hydrolysis forms Sol A.2.53 g citric acids are mixed with 1.12 g ethylene glycol, adds a small amount of dissolve with ethanol, after esterification, obtain citric acid glycol ester; Be dissolved in distilled water, then added 0.26 g p-Chlorobenzoic acid amide, obtained solution B.Mixing A and B solution, underpressure distillation, dehydration forms denseer jelly, and dry, roasting 5 h under 800 ° of C, obtains precursor powder thereupon.Take 1.00 g precursor powder, containing in the autoclave of formamide soln, react 8 h under 150 ° of C, suction filtration is separated, deionized water, washing with alcohol, and dry, roasting 2 h under 700 ° of C, obtains laminated perovskite Ca thereupon
3ti
2o
7powder.
Claims (6)
1. a low temperature preparation method for laminated perovskite, it is characterized in that the method successively step be:
1) by La
3+, Ce
3+, Sr
2+, Ca
2+, Ba
2+one or more salt and Mn
2+, Co
2+, Ni
2+, Zr
4+, Ti
4+one or more salt mix water-soluble formation solution A, by the chlorine source containing chlorion and the common water-soluble formation solution B of coordination agent, described coordination agent is one or more of PVA after citric acid, EDTA, glycine, degraded and citric acid glycol ester; Mixing A and B solution, stir, dehydration, dry, the precursor powder of calcining acquisition containing chlorion;
2) in a kettle., under alkaline condition, hydro-thermal or solvent heat treatment are carried out to precursor powder, after filtration, washing, drying, calcining, obtain target product and Ruddlesden-Popper type laminated perovskite.
2. the method for claim 1, the chlorine-containing compound that it is characterized in that as chlorine source is one or more of the hydrochloride of metal, p-Chlorobenzoic acid amide and ammonium chloride.
3. the method for claim 1, is characterized in that the calcining temperature of precursor is 600 ° of C ~ 1100 ° C.
4. the method for claim 1, is characterized in that basic solution precursor being carried out to hydro-thermal or solvent heat treatment is NH
4hCO
3, (NH
4)
2cO
3, NH
3h
2o, K
2cO
3, methane amide, trolamine, pyridine, aniline, quadrol, one or more water formed of anionite-exchange resin, ethanol or ethylene glycol solutions.
5. the method for claim 1, is characterized in that the temperature of precursor being carried out to hydrothermal treatment consists or solvent heat treatment is 80 ° of C ~ 220 ° C.
6. the method for claim 1, is characterized in that the calcining temperature of final product is 600 ° of C ~ 1100 ° C.
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CN108671926A (en) * | 2018-04-02 | 2018-10-19 | 河北科技大学 | The preparation method of one type Ruddlesden-Popper type Ca-Ti ore type catalysis materials |
CN110002851A (en) * | 2019-04-04 | 2019-07-12 | 安阳师范学院 | A kind of laminated perovskite Ca3Mn2O7The preparation method of ceramic material |
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