CN1974886A - Prepn process of nanometer rod and micron block of monocrystalline perovskite type oxide La1-xSrxMnO3 - Google Patents
Prepn process of nanometer rod and micron block of monocrystalline perovskite type oxide La1-xSrxMnO3 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims description 15
- 229910002075 lanthanum strontium manganite Inorganic materials 0.000 title abstract 3
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 8
- 229910052748 manganese Inorganic materials 0.000 claims description 8
- 239000011572 manganese Substances 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims 7
- 229910052751 metal Inorganic materials 0.000 claims 4
- 239000002184 metal Substances 0.000 claims 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims 3
- 229910002651 NO3 Inorganic materials 0.000 claims 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 2
- 239000012266 salt solution Substances 0.000 claims 2
- 159000000008 strontium salts Chemical class 0.000 claims 2
- 229910052692 Dysprosium Inorganic materials 0.000 claims 1
- 229910052693 Europium Inorganic materials 0.000 claims 1
- 229910052688 Gadolinium Inorganic materials 0.000 claims 1
- 229910052689 Holmium Inorganic materials 0.000 claims 1
- 229910052779 Neodymium Inorganic materials 0.000 claims 1
- 229910052772 Samarium Inorganic materials 0.000 claims 1
- 229910052804 chromium Inorganic materials 0.000 claims 1
- 229910052802 copper Inorganic materials 0.000 claims 1
- 229910052742 iron Inorganic materials 0.000 claims 1
- 150000002603 lanthanum Chemical class 0.000 claims 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims 1
- 229910052759 nickel Inorganic materials 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 2
- 239000004449 solid propellant Substances 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract 2
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 6
- 239000002071 nanotube Substances 0.000 description 5
- 229910002148 La0.6Sr0.4MnO3 Inorganic materials 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 4
- 229910003367 La0.5Sr0.5MnO3 Inorganic materials 0.000 description 3
- 238000001106 transmission high energy electron diffraction data Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005287 template synthesis Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920006289 polycarbonate film Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011175 product filtration Methods 0.000 description 1
- 238000004098 selected area electron diffraction Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
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Abstract
The preparation process of nanometer rod and micron block of monocrystalline perovskite type oxide La1-xSrxMnO3 belongs to the field of catalysis technology. The present invention prepares nanometer rod and micron block of monocrystalline perovskite type oxide La1-xSrxMnO3 directly in hydrothermal condition and by means of ultrasonic dispersion and controlling KOH amount, hydrothermal temperature and hydrothermal time without need of high temperature ignition. The preparation process can obtain nanometer rod of 50-850 nm diameter and 0.2-11 micron length and micron block of 1.0-11 micron edge length, and possesses latent application in multiphase catalysis, solid fuel cell, solid resistor, and other material fields.
Description
Technical field
The present invention relates to the preparation method of a kind of perovskite composite oxide nanometer rod and micron block monocrystalline, relate in particular to and utilize hydrothermal synthesis method to prepare monocrystalline perovskite type compound oxide La
1-xSr
xMnO
3The method of (x=0.4,0.5,0.6) nanometer rod and micron block.
Background technology
In the composite oxides of studying, perofskite type oxide is particularly noticeable.By the method for " cutting out ", people can design the perovskite Composite Oxides Materials of physical propertys such as having light, heat, electricity, magnetic and chemical propertys such as activation adsorption molecule, redox.Thereby solid electrolyte, chemical sensor, heat material, solid fuel cell and catalyzer etc. have been widely used as.
Traditional method for preparing perovskite composite oxide has sol-gel method, coprecipitation method, microemulsion method, template synthesis method etc., but the La that makes by these methods
1-xSr
xMnO
3Presoma must can obtain having single-phase perovskite crystal structure behind high temperature sintering, the specific surface area of gained particle is all less usually.Although the template synthesis method helps realizing largely the control to particle morphology, grain size and distribution thereof, but be subjected to the restriction of the character of template own.For example, (Appl Phys Lett, 2003,83 (25): 5427) the polyester template that adopts the pitting lithography to obtain has synthesized La to Levy etc.
0.325Pr
0.300Ca
0.375MnO
3Nanotube, external diameter are 800nm, and length is 4 μ m, and wall thickness is less than 100nm, and tube wall is made up of the crystal grain of about 20nm.(J Solid State Chem such as Leyva, 2004, be template 177:3949) with the porous polycarbonate film, utilize the microwave-assisted denitration technology, select suitable time and energy to guarantee that can slough nitrate radical does not damage masterplate again, has obtained perovskite type crystal structure La with the gained presoma then after 800 ℃ of calcinations
0.325Pr
0.300Ca
0.375MnO
3Nanotube.Wherein template used aperture is 1 μ m, and thickness is 8 μ m, and the nanotube external diameter of gained is 800nm, length is about 4 μ m, and thickness of pipe is 150nm, is that the nano particle of 20～50nm is formed by particle diameter, the external diameter of nanotube is less than the aperture of template, and the gained nanotube walls is thick relatively partially.When to adopt the aperture be template below the 1 μ m, obtain the nano wire of the about 10nm of diameter.This explanation, the aperture of template is to the pattern important influence of final product.Preparation technology is loaded down with trivial details for these hard template method, the cost height.Up to date, (Appl.Phys.Lett., 2002,80 (9) such as Zhu
1634) and Liu etc. (Mater.Res.Bull., 2003,38:817) adopt hydrothermal synthesis method, under different hydrothermal temperatures, prepared single-phase cubic perovskite La
0.5Sr
0.5MnO
3Nano wire and La
0.5Ba
0.5MnO
3Micron block.(Nano.Lett., 2004,4 (8): 1547) adopt similar method to make La such as Urban
0.7Ba
0.3MnO
3The nanometer piece.But perofskite type oxide La for different strontium doping amounts
1-xSr
xMnO
3The preparation of nanometer rod and micron block is especially at catalyzed oxidation hydrocarbon polymer and the outstanding La of oxygen-containing organic compound catalytic performance
0.6Sr
0.4MnO
3The preparation of catalyst nano rod and micron block there is no report at present.And according to the method that the present invention describes, handle by ultrasonic dispersing, control KOH consumption, hydrothermal temperature and hydro-thermal time, need not nano bar-shape and the block monocrystalline perovskite type compound oxide La of micron that high temperature sintering can obtain the different size size
1-xSr
xMnO
3(x=0.4,0.5,0.6).
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of perovskite composite oxide nanometer rod and micron block monocrystalline, the product that the present invention prepares is good perovskite composite oxide nanometer rod of degree of crystallinity and micron block monocrystal particle.
The preparation method of perovskite typed mixture nanometer rod provided by the invention and micron block monocrystalline, under agitation condition, with mol ratio be 3: 7 potassium permanganate and and the soluble metallic salt of manganese be the manganese source, with La, the soluble metallic salt of Sr is a raw material, with KOH is precipitation agent, KOH is added to by manganese source and La, in the mixing solutions that the soluble metallic salt of Sr is formed, form precipitation, after continuing to stir, be transferred to ultrasonic dispersing in the ultrasonic cleaner, it is transferred in the stopping property reactor, put into again in the thermostat container in 220～270 ℃ of insulation 24～72h, naturally cooling filters the product that obtains afterwards, deionized water wash, dry, grinding obtains black powder.
Gained black powder product is characterized with D8 ADVANCE type X-ray diffractometer (XRD), JEOL JSM6500F type high resolution scanning electron microscope (HRSEM), JEOL-2010 type transmission electron microscope (TEM) and selected area electron diffraction technology such as (SAED).The result shows that adopting the obtained sample of present method is diameter 50～850nm, and long 0.2～11 μ m nano bar-shape and rib length are the block monocrystalline perovskite type compound oxide La of 1.0～11 μ m microns
1-xSr
xMnO
3(contain micro-La (OH) in a few sample
3Dephasign).
Description of drawings
For further understanding the present invention, elaborate with embodiment below, and provide accompanying drawing and describe a nano bar-shape and the block monocrystalline perovskite type compound oxide La of micron that the present invention obtains
1-xSr
xMnO
3, wherein:
Fig. 1 is La
1-xSr
xMnO
3The XRD spectra of sample, wherein curve (a) La
0.4Sr
0.6MnO
3Embodiment 1; (b) La
0.5Sr
0.5MnO
3Embodiment 2; (c) La
0.6Sr
0.4MnO
3Embodiment 3; (d) La
0.6Sr
0.4MnO
3Embodiment 4;
Fig. 2 (a), (c) are respectively La
0.4Sr
0.6MnO
3The HRSEM of embodiment 1 sample and TEM photo, Fig. 2 (b), (d) are respectively La
0.6Sr
0.4MnO
3The HRSEM of embodiment 4 samples and TEM photo, wherein the illustration among Fig. 2 (c), (d) is respectively the SAED pattern of this sample.
Fig. 3 (a) and (b) are respectively La
0.5Sr
0.5MnO
3The HRSEM of embodiment 2 samples and TEM photo, wherein the illustration among Fig. 3 (b) is the SAED pattern of this sample.
Fig. 4 (a) and (b) are respectively La
0.6Sr
0.4MnO
3The HRSEM of embodiment 3 samples and TEM photo, wherein the illustration among Fig. 4 (b) is the SAED pattern of this sample.
Embodiment
Concrete implementation step of the present invention is as follows:
Embodiment 1: under normal temperature, normal pressure and magnetic agitation condition, with 0.003mol KMnO
4Be dissolved in the 30ml deionized water, after continuing to stir 10min, in above-mentioned solution, add 0.007mol MnCl
24H
2O continues to stir 15min, adds 0.004La (NO in above mixing solutions
3)
36H
2O and 0.006molSr (NO
3)
2Continue to stir 15min, 0.2333mol KOH is slowly joined in the above-mentioned mixing solutions, after continuing to stir 1h, be transferred in the ultrasonic cleaner, behind the ultrasonic dispersing 1h, it is transferred to (60% volume loading level) in the stainless steel cauldron that liner is a tetrafluoroethylene, put into again in the thermostat container in 250 ℃ of insulation 50h, naturally cool to room temperature afterwards, with the product filtration that obtains, deionized water wash 4～5 times, dry (120 ℃, 12h), grind that to obtain rib length be the block single crystal perovskite type oxide La of 5～11 μ m microns
0.4Sr
0.6MnO
3
Embodiment 2: under normal temperature, normal pressure and magnetic agitation condition, with 0.003mol KMnO
4Be dissolved in the 30ml deionized water, after continuing to stir 10min, in above-mentioned solution, add 0.007mol MnCl
24H
2O continues to stir 15min, adds 0.005La (NO in above mixing solutions
3)
36H
2O and 0.005molSr (NO
3)
2Continue to stir 15min, 0.2900mol KOH is slowly joined in the above-mentioned mixing solutions, after continuing to stir 1h, be transferred in the ultrasonic cleaner, behind the ultrasonic dispersing 1h, it is transferred to (60% volume loading level) in the stainless steel cauldron that liner is a tetrafluoroethylene, put into again in the thermostat container in 220 ℃ of insulation 72h, naturally cool to room temperature afterwards, the product that obtains is filtered, deionized water wash 4～5 times, dry (120 ℃, 12h), grinding obtains diameter 50～850nm, the block single crystal perovskite type oxide La of long 1.1～4.5 μ m microns of long 0.6～8.5 μ m nano bar-shape and rib
0.5Sr
0.5MnO
3
Embodiment 3: under normal temperature, normal pressure and magnetic agitation condition, with 0.003mol KMnO
4Be dissolved in the 30ml deionized water, after continuing to stir 10min, in above-mentioned solution, add 0.007molMn (CH
3COO)
24H
2O continues to stir 15min, adds 0.006La (NO in above mixing solutions
3)
36H
2O and 0.004mol Sr (NO
3)
2Continue to stir 15min, 0.3500mol KOH is slowly joined in the above-mentioned mixing solutions, after continuing to stir 1h, be transferred in the ultrasonic cleaner, behind the ultrasonic dispersing 1h, it is transferred to (60% volume loading level) in the stainless steel cauldron that liner is a tetrafluoroethylene, put into again in the thermostat container in 250 ℃ of insulation 50h, naturally cool to room temperature afterwards, the product that obtains is filtered, deionized water wash 4～5 times, dry (120 ℃, 12h), grinding obtains diameter 70～470nm, the block single crystal perovskite type oxide La of long 1.0～5.5 μ m microns of long 0.2～11 μ m nano bar-shape and rib
0.6Sr
0.4MnO
3(contain micro-La (OH) in the sample
3Dephasign).
Embodiment 4: under normal temperature, normal pressure and magnetic agitation condition, with 0.003mol KMnO
4Be dissolved in the 30ml deionized water, after continuing to stir 10min, in above-mentioned solution, add 0.007mol MnCl
24H
2O continues to stir 15min, adds 0.006La (NO in above mixing solutions
3)
36H
2O and 0.004molSr (NO
3)
2Continue to stir 15min, 0.3500mol KOH is slowly joined in the above-mentioned mixing solutions, after continuing to stir 1h, be transferred in the ultrasonic cleaner, behind the ultrasonic dispersing 1h, it is transferred to (60% volume loading level) in the stainless steel cauldron that liner is a tetrafluoroethylene, put into again in the thermostat container in 270 ℃ of insulation 24h, naturally cool to room temperature afterwards, the product that obtains is filtered, deionized water wash 4～5 times, dry (120 ℃, 12h), grinding obtains diameter 200～420nm, the block single crystal perovskite type oxide La of long 1.5～5.5 μ m microns of long 0.7～6.5 μ m nano bar-shape and rib
0.6Sr
0.4MnO
3(contain micro-La (OH) in the sample
3Dephasign).
Claims (4)
1. monocrystalline perovskite type compound oxide La
1-xSr
xMnO
3Nanometer rod and micron block preparation method, x is 0.4,0.5 and 0.6, it is characterized in that, under agitation condition, with mol ratio be 3: 7 potassium permanganate and and the soluble metallic salt of manganese be the manganese source, with La, the soluble metallic salt of Sr is a raw material, with KOH is precipitation agent, KOH is added to by manganese source and La, in the mixing solutions that the soluble metallic salt of Sr is formed, form precipitation, after continuing to stir, be transferred to ultrasonic dispersing in the ultrasonic cleaner, it is transferred in the stopping property reactor, put in the thermostat container in 220～270 ℃ of insulation 24～72h, naturally cooling filters the product that obtains afterwards again, deionized water wash, dry, grinding obtains nano bar-shape and the block perofskite type oxide La of micron
1-xSr
xMnO
3
2. preparation method according to claim 1 is characterized in that, described manganese source is hydrochloride, acetate, vitriol or the nitrate of potassium permanganate and manganese; Described soluble metal lanthanum salt is nitrate, acetate or hydrochloride; Described soluble metal strontium salt is nitrate, acetate.
3. preparation method according to claim 1 is characterized in that, described soluble metal lanthanum concentration of salt solution is 0.13～0.20mol/L; Described soluble metal strontium salt solution concentration is 0.13～0.20mol/L; Described potassium hydroxide solution concentration is 7.77～14.59mol/L.
4. preparation method according to claim 1 is characterized in that, described method can be applied to other perovskite composite oxides ABO
3And perovskite-like type composite oxides A
2BO
4The preparation of nanometer rod and micron block, wherein A is Nd, Sm, Eu, Gd, Dy, Ho, Er, B is Cr, Fe, Ni, Cu.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610114432 CN1974886A (en) | 2006-11-10 | 2006-11-10 | Prepn process of nanometer rod and micron block of monocrystalline perovskite type oxide La1-xSrxMnO3 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610114432 CN1974886A (en) | 2006-11-10 | 2006-11-10 | Prepn process of nanometer rod and micron block of monocrystalline perovskite type oxide La1-xSrxMnO3 |
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| Publication Number | Publication Date |
|---|---|
| CN1974886A true CN1974886A (en) | 2007-06-06 |
Family
ID=38125226
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|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103623832A (en) * | 2013-12-09 | 2014-03-12 | 河北工业大学 | Preparation method of rare-earth oxide material containing tourmaline |
| CN104437472A (en) * | 2014-11-06 | 2015-03-25 | 燕山大学 | Perovskite nanorod/graphene composite material and preparation method thereof |
| CN105540673A (en) * | 2016-01-29 | 2016-05-04 | 宁波工程学院 | Strontium manganate nanowires and microwires and preparation method thereof |
| CN109368705A (en) * | 2018-12-20 | 2019-02-22 | 西安工业大学 | A kind of TbMn1-xFexO3Raw powder's production technology |
| CN114243032A (en) * | 2021-12-03 | 2022-03-25 | 郑州佛光发电设备有限公司 | Preparation method and application of aluminum-air battery perovskite bimetallic oxide composite electrocatalyst |
-
2006
- 2006-11-10 CN CN 200610114432 patent/CN1974886A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103623832A (en) * | 2013-12-09 | 2014-03-12 | 河北工业大学 | Preparation method of rare-earth oxide material containing tourmaline |
| CN104437472A (en) * | 2014-11-06 | 2015-03-25 | 燕山大学 | Perovskite nanorod/graphene composite material and preparation method thereof |
| CN104437472B (en) * | 2014-11-06 | 2016-08-24 | 燕山大学 | A kind of perovskite nanometer rods/graphene composite material and preparation method |
| CN105540673A (en) * | 2016-01-29 | 2016-05-04 | 宁波工程学院 | Strontium manganate nanowires and microwires and preparation method thereof |
| CN105540673B (en) * | 2016-01-29 | 2019-01-25 | 宁波工程学院 | A kind of strontium manganate nano wire and micro wire and preparation method thereof |
| CN109368705A (en) * | 2018-12-20 | 2019-02-22 | 西安工业大学 | A kind of TbMn1-xFexO3Raw powder's production technology |
| CN114243032A (en) * | 2021-12-03 | 2022-03-25 | 郑州佛光发电设备有限公司 | Preparation method and application of aluminum-air battery perovskite bimetallic oxide composite electrocatalyst |
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