CN101412542A - Method for preparing perovskite type LaFe0.5Mn0.5O3 by geoceric acid solution combustion method - Google Patents
Method for preparing perovskite type LaFe0.5Mn0.5O3 by geoceric acid solution combustion method Download PDFInfo
- Publication number
- CN101412542A CN101412542A CNA2008101806698A CN200810180669A CN101412542A CN 101412542 A CN101412542 A CN 101412542A CN A2008101806698 A CNA2008101806698 A CN A2008101806698A CN 200810180669 A CN200810180669 A CN 200810180669A CN 101412542 A CN101412542 A CN 101412542A
- Authority
- CN
- China
- Prior art keywords
- stearic acid
- lafe
- temperature
- powder
- nitrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a method for preparing superfine perovskite type LaFe0.5Mn0.5O3 by a stearic acid solution combustion method. The method comprises the following proposal: respectively weighing lanthanum nitrate, ferric nitrate, manganese chloride and the stearic acid according to mol ratio of 1 to 0.5 to 0.5 to 7-10; dissolving the lanthanum nitrate, the ferric nitrate and the manganese chloride solids in the melted stearic acid at a temperature of between 110 and 117 DEG C to form stearic acid complex solution with enough reaction time; placing the solution in a muffle at a temperature of between 300 and 500 DEG C, and combusting the solution to obtain mixed oxide; and obtaining nanometer LaFe0.5Mn0.5O3 powder after calcining the mixture in the muffle at 600 DEG C for 1 hour. The crystallization degree of the obtained powder can be higher if the calcination temperature is higher.
Description
Technical field
The invention belongs to perovskite typed nanometer LaFe
0.5Mn
0.5O
3Preparing technical field specifically is to prepare perovskite typed nanometer LaFe with the stearic acid solution combustion method
0.5Mn
0.5O
3
Background technology
In recent years, nano science and nanotechnology were surging forward.Nano material is in magnetic, electronics, optics, highdensity sintering, photochemical catalysis, sensing, especially all have wide application prospect in the fields such as biology, medical science.
LaFe
0.5Mn
0.5O
3Belong to perovskite-type rare-earth composite oxides, at present it as the three-way catalyst of vehicle exhaust by scientific worker's broad research.Well-known synthetic method often greatly influences and changes the physical and chemical performance of material.Preparation LaFe
0.5Mn
0.5O
3Method less, only report has sol-gel method and two kinds of methods of pulsed laser deposition.Sol-gel processing prepares Nano compound to have: (1) temperature of reaction is low, and reaction process is easy to control; (2) uniformity coefficient of goods, purity height (homogeneity can reach molecule or atomic level); (3) stoichiometry is accurate, is easy to modification, adulterated wide ranges (comprising adulterated amount and kind).But the preparation required time is longer, is difficult for realizing industrialization.And pulse laser sediment method obviously exists shortcomings such as production cost is big.
Combustion synthesis method is synthetic and propose with respect to self propagating high temperature.The ultimate principle of this technology is: used oxygenant and fuel mixture have exothermic character, bring out the spontaneous generation redox reaction of energy down in certain temperature, finally obtain desired product.The globule size of products obtained therefrom and distribution etc. and fuel used kind, synthesis condition etc. all have much relations.
Present gel-burning synthetic method commonly used is a kind of low-temperature burning chemical process that sol-gel wet-chemical synthesis method and self-propagating combustion synthesis method are organically combined.This method at first generates gel in water solution system, burn its gel then and prepare compound.Have fast simply, convenient, and easily realize characteristics such as industrialization.Present low-temperature combustion method prepares compound and the employed organic-fuel of hotchpotch is a Padil, glycine etc.Because gel is to form in water solution system, so the shortcoming of the thing metal ion facile hydrolysis that can react inevitably, the products obtained therefrom granularity is bigger.
The stearic acid solution combustion method that we adopted is based on stearic acid fusing point lower (68-70 ℃), itself can be used as the solvent of metal-salt, and stearic acid has the dual function of Synergist S-421 95 and tensio-active agent concurrently, in building-up process, there is not or have only less water to participate in, thereby prevented the hydrolytic precipitation of metal ion, can reduce the agglomeration of product.The solid particulate that a large amount of gas percussions that produce in the combustion processes in addition form both can make powder granularity diminish, and also can prevent the reunion between the particle.So it is even to make size distribution under suitable condition, the nano-powder that particle diameter is little is expected to improve greatly the various physical and chemical performances of product.
Summary of the invention
The present invention has overcome the shortcoming of gel combustion method in the present water solution system, utilizes the characteristic of stearic acid non-aqueous solvent, has prepared perovskite typed nanometer LaFe with stearic solution combustion method
0.5Mn
0.5O
3, and preparation nanometer LaFe is provided
0.5Mn
0.5O
3Optimal conditions.
The present invention adopts with following scheme to realize: dissolve stearic acid under the constant temperature oil bath heating condition (1); (2) with lanthanum nitrate, iron nitrate, Manganous chloride tetrahydrate solid are dissolved in the fusion stearic acid, under the constant temperature magnetic agitation, and the control certain temperature, the chien shih reaction system becomes the stearic acid complex solution when reacting enough; (3) the stearic acid complex solution is burnt at a certain temperature and obtain mixed oxide, take out product and grind, put it in the retort furnace, calcine certain hour at a certain temperature, can obtain nanometer LaFe
0.5Mn
0.5O
3Powder.
The stearic acid solution combustion method prepares perovskite typed nanometer LaFe
0.5Mn
0.5O
3Suitable condition be: 1: 0.5: 0.5 in molar ratio: 7～1: 0.5: 0.5: 10 weighing lanthanum nitrate, iron nitrate, Manganous chloride tetrahydrate, stearic acid.Under the oil bath heating condition, earlier with the stearic acid dissolving, under the constant temperature magnetic agitation, with lanthanum nitrate, iron nitrate, Manganous chloride tetrahydrate solid are dissolved in the fusion stearic acid, 110～117 ℃ of temperature controls make it generate even stearic acid complex solution, are placed in the retort furnace, in 300-500 ℃ make its burning after, the taking-up product grinds, again in retort furnace in 600 ℃ of calcining 1h, can get nanometer LaFe
0.5Mn
0.5O
3Powder.Experimental result shows: calcining temperature is high more, and the crystallization degree of gained powder is better.
Lanthanum nitrate, iron nitrate, Manganous chloride tetrahydrate and stearic mol ratio influence granularity, purity and the pattern of powder.When lanthanum nitrate: iron nitrate: Manganous chloride tetrahydrate: stearic mol ratio Ψ=1: 0.5: 0.5: Ψ=1: 0.5: 0.5: in the time of (7-10), temperature control 110-117 ℃, stearic acid complex compound temperature of combustion is under 300-500 ℃, the mixed oxide of direct burning gained calcined 1 hour in 600 ℃ of retort furnaces after, can get nanometer LaFe
0.5Mn
0.5O
3Powder.Experimental result sees Table 1.By table 1 as seen: when the stearic acid amount is crossed when low, owing to lack enough complexing agent molecules, all complexings of reactant, the powder granularity skewness of preparation, the increase of powder reuniting degree; The stearic acid amount is big more, and the products obtained therefrom particle diameter is more little.The reason that reduces can think that it is more tiny that this helps powder granularity owing to along with the increasing of stearic acid add-on, generated more gas.But the stearic acid amount is too high, and can make has more organic substance residues in the final product, for removing organism, needs the calcining longer time.Can cause waste on the other hand.So should select lanthanum nitrate, iron nitrate for use, Manganous chloride tetrahydrate and stearic mol ratio are to be advisable in 1: 1: 7～1: 1: 10.
Table 1 lanthanum nitrate, iron nitrate, Manganous chloride tetrahydrate, stearic mol ratio and LaFe
0.5Mn
0.5O
3The relation of powder granularity size
| Ψ | 6 | 7 | 8 | 10 |
| Size distribution and pattern | Pattern is irregular, and agglomeration is obvious | 30nm-60nm nanometer aggregate | 20nm-50nm nanometer aggregate | 18nm-45nm nanometer aggregate |
Temperature control is 110～117 ℃ in the oil bath, is because react in water bath with thermostatic control, and length not only consuming time (generally more than 12 hours) and reaction are not exclusively.As reaction conditions, between 110～117 ℃ of the temperature controls, reaction can be finished with fast speeds with oil bath.
It is because stearic acid complex compound sample is put into retort furnace that temperature of combustion is controlled to be 300-500 ℃, begins to heat up.When temperature reaches 300 ℃, rapidly catching fire, concentrate, be 4～6 minutes combustion time.Too high muffle furnace must consume too many energy, so temperature of combustion is controlled between 300-500 ℃.
Experiment is found: the powder after the burning is a mixed oxide, in the retort furnace in 600 ℃ of calcinings after 1 hour, mixed oxide is transformed into perovskite typed nanometer LaFe
0.5Mn
0.5O
3Powder.The incinerating temperature is high more, forms LaFe
0.5Mn
0.5O
3Crystallization degree is higher, but the specific surface area of powder will inevitably reduce.The XRD of gained powder and sem photograph are seen accompanying drawing 1-3.
The present invention has following advantage and effect:
Raw material used in the present invention is easy to get, and nontoxic.The technology that is adopted has fast simple, and is convenient, and easily realize characteristics such as industrialization.Owing to use the stearic acid that can produce a large amount of gases, make the products obtained therefrom even particle size distribution, size distribution is little.
Description of drawings
Fig. 1 is as lanthanum nitrate, iron nitrate, Manganous chloride tetrahydrate and stearic mol ratio (nLa (NO3) 3: nFe (NO3) 3: be 1: 0.5: 0.5 nMnCl2: nCH3-(CH2) 16-COOH): 8, under 115 ℃ of the oil bath temperature controls, the stearic acid complex solution that is generated is at powder after 500 ℃ of burnings and at the X-ray diffracting spectrum of 600 ℃ of retort furnaces calcining gained powder after 1 hour.Fig. 1 a is the XRD of burning back mixed oxide, and Fig. 1 b is at the gained perovskite typed nanometer LaFe after 600 ℃ of retort furnaces are calcined 1 hour of powder after the burning
0.5Mn
0.5O
3The X-ray diffracting spectrum of powder.
Fig. 2 is lanthanum nitrate, iron nitrate, Manganous chloride tetrahydrate, stearic mol ratio is 1: 0.5: 0.5: 8, under 115 ℃ of the temperature controls, the stearic acid complex solution that makes generation is 500 ℃ of burnings, and the product after the burning is at 600 ℃ of sem photographs of calcining 1 hour gained powder down.
Fig. 3 is as lanthanum nitrate, iron nitrate, Manganous chloride tetrahydrate and stearic mol ratio (nLa (NO3) 3: nFe (NO3) 3: be 1: 0.5: 0.5 nMnCl2: nCH3-(CH2) 16-COOH): 7, under 113 ℃ of the oil bath temperature controls, the stearic acid complex solution that is generated is at powder after 450 ℃ of burnings and at 700 ℃ of retort furnaces calcining gained perovskite typed nanometer LaFe after 1 hour
0.5Mn
0.5O
3X-ray diffracting spectrum.
Embodiment
Embodiment 1
A certain amount of lanthanum nitrate of difference weighing, iron nitrate, Manganous chloride tetrahydrate, stearic acid, making its mol ratio is 1: 0.5: 0.5: 8.At first under the constant temperature oil bath heating condition, with the stearic acid dissolving, under the constant temperature magnetic agitation, with lanthanum nitrate, iron nitrate, Manganous chloride tetrahydrate solid are dissolved in the fusion stearic acid, 115 ℃ of temperature controls, when reacting enough chien shih its become the stearic acid complex solution.Make it 500 ℃ of burnings, the product that takes out after burning grinds and puts it in the retort furnace, calcines 1 hour down at 600 ℃, obtains nanometer LaFe as depicted in figs. 1 and 2
0.5Mn
0.5O
3It is spherical that powder, the pattern of powder are approximately, the nanometer aggregate of size about 20nm-50nm.
Embodiment 2
A certain amount of lanthanum nitrate of difference weighing, iron nitrate, Manganous chloride tetrahydrate, stearic acid, making its mol ratio is 1: 0.5: 0.5: 7.At first under the constant temperature oil bath heating condition, stearic acid is dissolved, in the constant temperature magnetic agitation, with lanthanum nitrate, iron nitrate, Manganous chloride tetrahydrate solid are dissolved in the fusion stearic acid, 113 ℃ of temperature controls, its generation stearic acid complex solution of chien shih after 450 ℃ of burnings, takes out it product grinding and also puts it in the retort furnace when reacting enough, calcined 1 hour down at 700 ℃, obtain nanometer LaFe
0.5Mn
0.5O
3Powder.The XRD diffractogram of powder is seen accompanying drawing 3.
Claims (1)
1. one kind prepares perovskite typed nanometer LaFe
0.5Mn
0.5O
3Method, adopt the stearic acid solution combustion method to prepare perovskite typed nanometer LaFe
0.5Mn
0.5O
3Its suitable preparation condition is: 1: 0.5: 0.5 in molar ratio: 7～1: 0.5: 0.5: 10, difference weighing lanthanum nitrate, iron nitrate, Manganous chloride tetrahydrate, stearic acid, under the oil bath heating condition, earlier stearic acid is dissolved, under the constant temperature magnetic agitation, with lanthanum nitrate, iron nitrate, the Manganous chloride tetrahydrate solid is dissolved in the fusion stearic acid, 110～117 ℃ of temperature controls, chien shih is after it generates stearic acid complex solution when reacting enough, be placed in the 300-500 ℃ of retort furnace, make its burning, the burning back is taken out product and is ground, again in retort furnace in 600 ℃ the calcining 1h, can get nano-perovskite type LaFe
0.5Mn
0.5O
3
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101806698A CN101412542A (en) | 2008-11-19 | 2008-11-19 | Method for preparing perovskite type LaFe0.5Mn0.5O3 by geoceric acid solution combustion method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101806698A CN101412542A (en) | 2008-11-19 | 2008-11-19 | Method for preparing perovskite type LaFe0.5Mn0.5O3 by geoceric acid solution combustion method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101412542A true CN101412542A (en) | 2009-04-22 |
Family
ID=40593313
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008101806698A Pending CN101412542A (en) | 2008-11-19 | 2008-11-19 | Method for preparing perovskite type LaFe0.5Mn0.5O3 by geoceric acid solution combustion method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101412542A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214057A (en) * | 2012-01-20 | 2013-07-24 | 中北大学 | Photocatalytic degradation of dinitrochlorobenzene waste water |
| CN103570078A (en) * | 2013-11-01 | 2014-02-12 | 中北大学 | Preparation method of nanoscale ferrite |
| CN104071845A (en) * | 2014-07-15 | 2014-10-01 | 渤海大学 | Preparation method for SLTON perovskite NOx powder |
| CN104071844A (en) * | 2014-07-15 | 2014-10-01 | 渤海大学 | Burning method for preparing Sr2YTaO6 powder |
| CN104085927A (en) * | 2014-07-18 | 2014-10-08 | 渤海大学 | Preparation method of LSTON (La, Sc, Ta, O and N) perovskite-type nitrogen oxide solid solution powder |
| CN104085924A (en) * | 2014-07-15 | 2014-10-08 | 渤海大学 | Method for preparing SLYTON perovskite type nitrogen oxide powder |
| CN107629790A (en) * | 2017-11-09 | 2018-01-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for LED blue light perovskite fluorescent material and products thereof and application |
| CN114408986A (en) * | 2022-01-21 | 2022-04-29 | 陕西彩虹新材料有限公司 | Nanoscale single crystal ternary cathode material and preparation method thereof |
-
2008
- 2008-11-19 CN CNA2008101806698A patent/CN101412542A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214057A (en) * | 2012-01-20 | 2013-07-24 | 中北大学 | Photocatalytic degradation of dinitrochlorobenzene waste water |
| CN103570078A (en) * | 2013-11-01 | 2014-02-12 | 中北大学 | Preparation method of nanoscale ferrite |
| CN103570078B (en) * | 2013-11-01 | 2014-12-10 | 中北大学 | Preparation method of nanoscale ferrite |
| CN104071844A (en) * | 2014-07-15 | 2014-10-01 | 渤海大学 | Burning method for preparing Sr2YTaO6 powder |
| CN104085924A (en) * | 2014-07-15 | 2014-10-08 | 渤海大学 | Method for preparing SLYTON perovskite type nitrogen oxide powder |
| CN104071845A (en) * | 2014-07-15 | 2014-10-01 | 渤海大学 | Preparation method for SLTON perovskite NOx powder |
| CN104071845B (en) * | 2014-07-15 | 2016-01-06 | 渤海大学 | A kind of SLTON perovskite typed oxynitride raw powder's production technology |
| CN104085924B (en) * | 2014-07-15 | 2016-01-20 | 渤海大学 | A kind of method preparing SLYTON perovskite typed oxynitride powder |
| CN104071844B (en) * | 2014-07-15 | 2016-01-20 | 渤海大学 | A kind of combustion method prepares the method for yttrium tantalic acid strontium powder |
| CN104085927A (en) * | 2014-07-18 | 2014-10-08 | 渤海大学 | Preparation method of LSTON (La, Sc, Ta, O and N) perovskite-type nitrogen oxide solid solution powder |
| CN104085927B (en) * | 2014-07-18 | 2016-03-09 | 渤海大学 | The preparation method of LSTON perovskite typed oxynitride solid-solution powder |
| CN107629790A (en) * | 2017-11-09 | 2018-01-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for LED blue light perovskite fluorescent material and products thereof and application |
| CN114408986A (en) * | 2022-01-21 | 2022-04-29 | 陕西彩虹新材料有限公司 | Nanoscale single crystal ternary cathode material and preparation method thereof |
| CN114408986B (en) * | 2022-01-21 | 2024-02-13 | 陕西彩虹新材料有限公司 | Nanoscale monocrystal ternary cathode material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101412542A (en) | Method for preparing perovskite type LaFe0.5Mn0.5O3 by geoceric acid solution combustion method | |
| Deganello et al. | Solution combustion synthesis, energy and environment: Best parameters for better materials | |
| CN109019701B (en) | Preparation method of rock salt type (MgCoCuNiZn) O high-entropy oxide powder material | |
| CN100558645C (en) | Ultra-fine perovskite type LaFeO 3And LaMnO 3A kind of preparation method | |
| US8546284B2 (en) | Process for the production of plasma sprayable yttria stabilized zirconia (YSZ) and plasma sprayable YSZ powder produced thereby | |
| CN106622241A (en) | Nano spinel type catalyst and preparation method thereof | |
| CN104108749B (en) | A kind of preparation method of strontium titanate doping | |
| CN103215104A (en) | Mixed metal oxide oxygen carrier and preparation method thereof | |
| CN105755541B (en) | A kind of method that combustion synthesis reaction synthesizing zinc oxide whisker is induced using microwave | |
| Banerjee et al. | Preparation of nanoparticles of oxides by the citrate–nitrate process: effect of metal ions on the thermal decomposition characteristics | |
| CN107129304A (en) | Method for synthesizing lanthanum molybdate-based electrolyte material in one step by microwave combustion-supporting method | |
| JP2017538262A (en) | Cathode material manufacturing method and special cathode material | |
| CN104353461A (en) | Preparation method of high-specific surface nanometer magnesium ferrite catalyst material capable of being used in solid propellant | |
| CN108339562B (en) | Preparation method of iron ion doped carbon nitride nanotube and obtained product | |
| CN100398453C (en) | Method of burning gel of stearic acid for preparing Nano LaCo03 in type of perovskite | |
| Zhang et al. | Preparation and characterization of pyrochlore oxide Y2Ti2O7 nanocrystals via gel-combustion route | |
| KR101143859B1 (en) | Synthesis of conductive zinc oxide by ultrasonic-spray pyrolysis process | |
| CN103011281A (en) | Method for synthesizing sphere-like nano yttrium and cerium doped zirconia according to ethylene glycol sol-gel method | |
| CN109865535B (en) | Metastable state cerium oxide or cerium-zirconium solid solution nano material | |
| CN104973624A (en) | Preparation method of meshy tetragonal phase zirconia nano powder | |
| Biswas et al. | Synthesis of nanocrystalline yttria doped ceria powder by urea–formaldehyde polymer gel auto-combustion process | |
| CN104326500B (en) | A kind of preparation method of fluffy state nano yttrium oxide powder | |
| CN103304228A (en) | Self-propagating combustion synthesis method for palladium-copper ferrite nano-powder | |
| CN109081694A (en) | Precursor liquid and high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder with and preparation method thereof | |
| Srisombat et al. | Chemical synthesis of magnesium niobate powders |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090422 |