CN102874860B - Method for preparing magnesium aluminate lanthanum powder through combustion method - Google Patents
Method for preparing magnesium aluminate lanthanum powder through combustion method Download PDFInfo
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- CN102874860B CN102874860B CN201210329510.4A CN201210329510A CN102874860B CN 102874860 B CN102874860 B CN 102874860B CN 201210329510 A CN201210329510 A CN 201210329510A CN 102874860 B CN102874860 B CN 102874860B
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- magnesium aluminate
- powder
- lanthanum
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Abstract
The invention relates to a method for preparing magnesium aluminate lanthanum (LaMgAl11O19) powder through a combustion method. The method is used for preparing magnesium aluminate lanthanum powder in shape of expansion powder by controlling the mixture ratio of raw materials and the pH (potential of hydrogen) of solution and setting the roasting temperature and constant-temperature roasting time after the self-propagating burning. The method comprises the steps as follows: mixing La(NO3)3/6H2O, Mg(NO3)2/6H2O, Al(NO3)3/9H2O and C2H5NO2 based on mol ratio of 1:1:11:(20 to 30) into a ceramic crucible; adding proper distilled water; heating the mixing solution to reach 70 DEG C through heating magnetic agitator; uniformly agitating; slowly dropping ammonia water to adjust the pH of the mixing solution to 2 to 4; arranging the mixing solution into a muffle furnace; and heating until the self-propagating burning is generated; and roasting for 3 to 6 hours at 1050 DEG C. According to the method provided by the invention, the reaction is conducted in a short time, and the burning air flow brings high impacting, so that particles can be refined conveniently, and the degree of agglomerating of particles which are the products of powder can be reduced.
Description
Technical field
The present invention relates to a kind of method that combustion method prepares lanthanum-magnesium aluminate powder, belong to the preparing technical field of lanthanum-magnesium aluminate powder.
Background technology
Magnesium base lanthanum hexaaluminate (LaMgAl
11o
19) namely lanthanum-magnesium aluminate (LMA) be lanthanum hexaaluminate (LaAl
11o
18) one in system, this structure be six sides and cube mixed structure, its stable in properties has excellent heat physical properties, so not only can be used in optical material, is also thermal barrier coating, conductivity ceramics, the study hotspot of CMP abrasive material.
At present, the method being used for preparing aluminate powder material is a lot, mainly contains atomizing freeze drying method, coprecipitation method and sol-gel method etc.Combustion synthesis method is adopted to be using soluble metallic salt (nitrate) and organic-fuel (as glycine, urea, citric acid etc.) as reactant, metal nitrate serves as oxygenant in the reaction, organic-fuel serves as reductive agent in the reaction, reaction system is lighted at a certain temperature and is caused violent redox reaction, along with the promotion of combustion wave, reactant changes final product into rapidly, and this shortens experimental period greatly.And the products distribution obtained is even, purity is high, and its lytic activity is high.The method technique is simple, and the energy expenditure adding equipment when can reduce roasting of incendiary material, lanthanum-magnesium aluminate prepared by the stoving oven of available lower-wattage, but the selection of incendiary material is most important, and the kind of incendiary material and add-on will directly affect the purity of powder.
The present invention adopts lanthanum nitrate hexahydrate (La (NO
3)
36H
2o), magnesium nitrate hexahydrate (Mg (NO
3)
26H
2o) and nine water aluminum nitrate (Al (NO
3)
39H
2o) be oxygenant, glycine (C
2h
5nO
2) as incendiary material and reductive agent, adopt combustion method to prepare lanthanum-magnesium aluminate powder, determine the optimum process condition preparing lanthanum-magnesium aluminate powder.
Summary of the invention
The object of this invention is to provide a kind of method that combustion method prepares lanthanum-magnesium aluminate powder, with the lanthanum-magnesium aluminate powder that the method is obtained, because the reaction times is short, the severe impact of combustion gas flowing, be conducive to the refinement of particle, reduce interparticle reunion degree, by controlling proportioning raw materials, solution ph, the lanthanum-magnesium aluminate powder of bulk shape can be prepared in conjunction with setting maturing temperature and roasting time after climing combustion.
For achieving the above object, the present invention by the following technical solutions: raw material is Al (NO
3)
39H
2o, La (NO
3)
3× 6H
2o, Mg (NO
3)
26H
2o and C
6h
14o
6.In combustion reactions, Al (NO
3)
39H
2o, La (NO
3)
36H
2o, Mg (NO
3)
26H
2o and C
2h
5nO
2mol ratio directly affect the purity of powder, according to the mol ratio of the thermochemical theory computing fuel (reductive agent) in propellant chemistry with nitrate (oxygenant).By calculating total reductive agent of raw material and oxygenant, using these two data as the stoichiometric coefficient of fuel and nitrate, suppose combustionmaterial perfect combustion, then product is CO
2, N
2and H
2o, the valency of Elements C, H is+4 valencys and+1 valency respectively, and element O valency is-divalent, and N is the neutral element of 0 valency.Calculate known La (NO
3)
36H
2total valency of O is-15, Al (NO
3)
39H
2total valency of O is-15, Mg (NO
3)
26H
2the valency of O is-10, belongs to oxygenant; Glycine C
2h
5nO
2total valency be+9 valencys, belong to reductive agent.Namely its theoretical molar ratio is:
La(NO
3)
3·6H
2O：Mg(NO
3)
2·6H
2O：Al(NO
3)
3·9H
2O ：C
2H
5NO
2= 1：1：11：21.11
Be 1:1:11:(20 ~ 30 by mol ratio) La (NO
3)
36H
2o, Mg (NO
3)
26H
2o, Al (NO
3)
39H
2o and C
2h
5nO
2be mixed in ceramic crucible, add appropriate distilled water, the magnetic stirring apparatus of mixing solutions band heating is heated to 70 DEG C and after stirring, slowly drip ammoniacal liquor and regulate the pH value of mixing solutions between 2 ~ 4, gained solution is precursor liquid.Crucible is put into retort furnace heat, when temperature is enough high, in precursor liquid, solvent evaporates gradually becomes gel, when reaching its ignition temperature, in retort furnace, there is self-propagating combustion reaction, reacting violent and being attended by a large amount of smoke creating, combustion processes terminates within tens seconds, continue at 1050 DEG C of roasting 3 ~ 6h, fully obtain bulk sprills product, i.e. lanthanum-magnesium aluminate powder in crucible after reaction.
The present invention has the following advantages compared with existing preparation technology:
1, have technique simple, preparation cycle is short, and equipment requirements is low, and productive rate is high, and the uniform feature of distribution of reaction products, easily realizes suitability for industrialized production.
2, the present invention is by controlling proportioning raw materials, solution ph, bulk pulverous lanthanum-magnesium aluminate powder can be prepared in conjunction with setting maturing temperature and constant temperature calcining time after climing combustion, because the reaction times is short, the severe impact of combustion gas flowing, be conducive to the refinement of particle, reduce interparticle reunion degree, control process easy handling.
Accompanying drawing explanation
Fig. 1 is the X-ray diffraction spectrogram of the lanthanum-magnesium aluminate powder prepared under the present embodiment.
embodiment
Embodiment 1
Weigh a certain amount of La (NO respectively
3)
36H
2o, Mg (NO
3)
26H
2o, Al (NO
3)
39H
2o and C
2h
5nO
2, their mol ratio is 1:1:11:20, is mixed in ceramic crucible, add appropriate distilled water, the magnetic stirring apparatus of mixing solutions band heating is heated to 70 DEG C and after stirring, slowly drip ammoniacal liquor and regulate the pH value of mixing solutions to be 4, gained solution is precursor liquid.Crucible is put into after retort furnace is heated to that self-propagating combustion reaction occurs and continues at 1050 DEG C of roasting 4h, obtain bulk sprills product, XRD spectra analytical results shows that product is lanthanum-magnesium aluminate.
Embodiment 2
Weigh a certain amount of La (NO respectively
3)
36H
2o, Mg (NO
3)
26H
2o, Al (NO
3)
39H
2o and C
2h
5nO
2, their mol ratio is 1:1:11:22, is mixed in ceramic crucible, add appropriate distilled water, the magnetic stirring apparatus of mixing solutions band heating is heated to 70 DEG C and after stirring, slowly drip ammoniacal liquor and regulate the pH value of mixing solutions to be 4, gained solution is precursor liquid.Crucible is put into after retort furnace is heated to that self-propagating combustion reaction occurs and continues at 1050 DEG C of roasting 4h, obtain bulk sprills product, XRD spectra analytical results shows that product is lanthanum-magnesium aluminate.
Embodiment 3
Weigh a certain amount of La (NO respectively
3)
36H
2o, Mg (NO
3)
26H
2o, Al (NO
3)
39H
2o and C
2h
5nO
2, their mol ratio is 1:1:11:24, is mixed in ceramic crucible, add appropriate distilled water, the magnetic stirring apparatus of mixing solutions band heating is heated to 70 DEG C and after stirring, slowly drip ammoniacal liquor and regulate the pH value of mixing solutions to be 3, gained solution is precursor liquid.Crucible is put into after retort furnace is heated to that self-propagating combustion reaction occurs and continues at 1050 DEG C of roasting 4h, obtain bulk sprills product, XRD spectra analytical results shows that product is lanthanum-magnesium aluminate.
Embodiment 4
Weigh a certain amount of La (NO respectively
3)
36H
2o, Mg (NO
3)
26H
2o, Al (NO
3)
39H
2o and C
2h
5nO
2, their mol ratio is 1:1:11:26, is mixed in ceramic crucible, add appropriate distilled water, the magnetic stirring apparatus of mixing solutions band heating is heated to 70 DEG C and after stirring, slowly drip ammoniacal liquor and regulate the pH value of mixing solutions to be 3, gained solution is precursor liquid.Crucible is put into after retort furnace is heated to that self-propagating combustion reaction occurs and continues at 1050 DEG C of roasting 6h, obtain bulk sprills product, XRD spectra analytical results shows that product is lanthanum-magnesium aluminate.
Embodiment 5
Weigh a certain amount of La (NO respectively
3)
36H
2o, Mg (NO
3)
26H
2o, Al (NO
3)
39H
2o and C
2h
5nO
2, their mol ratio is 1:1:11:28, is mixed in ceramic crucible, add appropriate distilled water, the magnetic stirring apparatus of mixing solutions band heating is heated to 70 DEG C and after stirring, slowly drip ammoniacal liquor and regulate the pH value of mixing solutions to be 3, gained solution is precursor liquid.Crucible is put into after retort furnace is heated to that self-propagating combustion reaction occurs and continues at 1050 DEG C of roasting 5h, obtain bulk sprills product, XRD spectra analytical results shows that product is lanthanum-magnesium aluminate.
Embodiment 6
Weigh a certain amount of La (NO respectively
3)
36H
2o, Mg (NO
3)
26H
2o, Al (NO
3)
39H
2o and C
2h
5nO
2, their mol ratio is 1:1:11:30, is mixed in ceramic crucible, add appropriate distilled water, the magnetic stirring apparatus of mixing solutions band heating is heated to 70 DEG C and after stirring, slowly drip ammoniacal liquor and regulate the pH value of mixing solutions to be 2, gained solution is precursor liquid.Crucible is put into after retort furnace is heated to that self-propagating combustion reaction occurs and continues at 1050 DEG C of roasting 3h, obtain bulk sprills product, XRD spectra analytical results shows that product is lanthanum-magnesium aluminate.
Claims (1)
1. prepare lanthanum-magnesium aluminate LaMgAl by combustion method for one kind
11o
19the method of powder, is characterized in that, raw material is La (NO
3)
36H
2o, Mg (NO
3)
26H
2o, Al (NO
3)
39H
2o and glycine C
2h
5nO
2, by the La (NO of suitable mol ratio
3)
36H
2o, Mg (NO
3)
26H
2o, Al (NO
3)
39H
2o and C
2h
5nO
2be mixed in ceramic crucible, add appropriate distilled water, the magnetic stirring apparatus of mixing solutions band heating is heated to proper temperature and after stirring, slow dropping ammoniacal liquor regulates the pH value of mixing solutions, be placed in retort furnace and be heated to self-propagating combustion occur and roasting at a certain temperature several hours, obtain bulk Powdered lanthanum-magnesium aluminate product;
La (NO
3)
36H
2o, Mg (NO
3)
26H
2o, Al (NO
3)
39H
2o and C
2h
5nO
2mol ratio be 1:1:11:(20 ~ 30);
The magnetic stirring apparatus of mixing solutions band heating is heated to 70 DEG C and after stirring, by dripping ammoniacal liquor, regulates the pH value of mixing solutions between 2 ~ 4;
Described maturing temperature is 1050 DEG C, roasting time 3 ~ 6h.
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|---|---|---|---|
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| CN104649872B (en) * | 2013-11-19 | 2016-08-17 | 中国石油天然气股份有限公司 | A kind of method of selectivity of light olefin oxidation |
| CN104649876B (en) * | 2013-11-19 | 2016-11-09 | 中国石油天然气股份有限公司 | A kind of preparation method of methacrylaldehyde |
| CN104528753B (en) * | 2015-01-10 | 2017-11-07 | 辽宁石油化工大学 | A kind of method that antifungin lanthanum powder is prepared with combustion method |
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Non-Patent Citations (2)
| Title |
|---|
| Combustion synthesis and characterization of nanocrystalline LaAlO3 powders;Zhong-Qing Tian et al.;《Materials Chemistry and Physics》;20071231;第106卷;126-129 * |
| 超细红色荧光粉LaMgAl11O19:Eu3+的制备与发光性能;莎仁等;《中国科学:化学》;20101231;第40卷(第4期);331-335 * |
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