CN108689423B - Monoclinic phase SmCO3(OH) preparation method of multilevel structure crystallite - Google Patents
Monoclinic phase SmCO3(OH) preparation method of multilevel structure crystallite Download PDFInfo
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- CN108689423B CN108689423B CN201811020458.8A CN201811020458A CN108689423B CN 108689423 B CN108689423 B CN 108689423B CN 201811020458 A CN201811020458 A CN 201811020458A CN 108689423 B CN108689423 B CN 108689423B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/247—Carbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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Abstract
The invention discloses a kind of monoclinic phase SmCO3(OH) first Sm (NO is added under agitation in hexa by the preparation method of multilevel structure crystallite3)3In solution, wherein Sm (NO3)3Molar ratio with hexa is (2:1) ~ (1:2)；Reaction precursor liquid is placed under the conditions of 160 ~ 200 DEG C of microwave hydrothermals and reacts 15 ~ 60min, generates precipitating, after reaction cooled to room temperature；It isolates precipitating and washs drying, obtain SmCO3(OH) multilevel structure crystallite.The present invention is with Sm (NO3)3For samarium source, multilevel structure SmCO is realized under the conditions of microwave hydrothermal3(OH) successful building；Short using the reaction time of microwave-hydrothermal method, instrument and equipment is simple, easy to operate, is easy to control；Obtained SmCO3(OH) purity is high, crystallinity of crystallite be strong, good dispersion.
Description
Technical field
The invention belongs to micro/nano material technical fields, more particularly to a kind of monoclinic phase SmCO3(OH) multilevel structure is micro-
Brilliant preparation method.
Background technique
Rare earth element has 4fx5d0-16s2Electronic structure, because its atomic radius is big and easily lose outer layer 6s, 5d or
4f electronics, and there is very strong activity, so that rare earth metal and its compound show typical light, electricity, magnetic and catalysis spy
Property.Specific micro-/ nano manufacturing technology is introduced into the preparation process of functional rareearth material, make the advantage of rare earth material with
The characteristic of micro/nano material combines, and obtained micro-/ nano rare earth material is in rare earth permanent-magnetic material, hydrogen storage material, catalysis material
The application of material, micro-/ nano rare earth phosphor and varistor etc. is not only expected to realize the upgrading of conventional industries, but also
The advantage that the added value of rare earth material will be promoted to utilize and further play China's rare earth resources has important research valence
Value and meaning.The rare earth metal subcarbonate of different-shape, such as fusiform CeOHCO3 [Zhao D L, Yang Q, Han
Z H, et al. Biomolecule-assisted Synthesis of Rare Earth Hydroxycarbonates
[J] Solid State Sciences, 2008,10:31-39.], dodecahedron shape NdOHCO3 [Xu Z Y, Zhang
Y J, Fang Z Y, et al. Controllable Synthesis and Optical Properties of
NdOHCO3 Dodecahedral Microcrystals [J]. Materials Research Bulletin, 2010,
45:74-79.] and dumbbell shaped PrOHCO3 [Zhao D L, Yang Q, Han Z H, et al. Rare Earth
Hydroxycarbonate Materials with Hierarchical Structures: Preparation and
Characterization, and Catalytic Activity of Derived Oxides [J]. Solid State
Sciences, 2008,10:1028-103.] etc. existing document report.
Pattern, size, crystal form and the exposure crystal face of inorganic semiconductor material have weight for its light, electricity, magnetic and chemical characteristic
The influence wanted.Basic carbonate samarium is widely used in electronics and ceramic industry as a kind of important lanthanide rare compound-material
Field.Because samarium is easily magnetized and is not easy demagnetization, basic carbonate samarium is expected to have in solid state electronic device and superconductor important
Application.In the preparation for being also widely used for samarium oxide as presoma using basic carbonate samarium.In addition, some researches show that Eu3+It mixes
Miscellaneous SmCO3(OH) it can be used for preparing utilization rate of the optical conversion film to improve light.Such as, SmCO octahedronlike3(OH) [Zhang
Y J, He H M, Yang X Z, et al. Morphology-controlled Synthesis,
Characterization, Growth Mechanism of SmCO3(OH) with High Uniform Size and
Photoluminescence Property of SmCO3(OH): Eu3+ [J]. Powder Technology, 2012,
224:175-182.] and diamond shape SmCO3(OH) [Yin X B, Zhang Y J, Fang Z Y, et al.
Hydrothermal Synthesis of Rhombus-like SmCO3OH Microplates and Its
Photoluminescence Property Doped with Eu3+ [J]. Chinese Journal of Chemical
Physics, 2010, 23: 102-106.].Currently reported SmCO3(OH) preparation method mostly uses hydro-thermal method, system
The standby period is long, and energy consumption is more, SmCO prepared by conventional hydrothermal method3It (OH) is mostly two-dimensional structure (such as diamond shape), the utilization to photon
Rate is relatively low, needs doping with rare-earth ions such as Eu3+To improve its optical property.
Summary of the invention
The purpose of the present invention is to provide a kind of monoclinic phase SmCO3(OH) preparation method of multilevel structure crystallite, solves
SmCO in the prior art3(OH) for diamond structure and long preparation period, energy consumption be more and the problem low to photon utilization rate.
The technical scheme adopted by the invention is that monoclinic phase SmCO3(OH) preparation method of multilevel structure crystallite, is specifically pressed
It is carried out according to following steps:
Step 1, under agitation by hexa be added Sm (NO3)3In solution, continues stirring 10min and formed instead
Answer precursor liquid；
Reaction precursor liquid is placed in microwave hydrothermal liner and reacts by step 2, generates precipitating, after reaction natural cooling
To room temperature；
Step 3 isolates the precipitating in step 2 and washs drying, obtains the flower-like structure SmCO that strip is self-assembled into3
(OH) crystallite.
Further, Sm (NO in the step 13)3The concentration of solution is 0.2 ~ 0.5molL-1, the pH of reaction precursor liquid
=8~9。
Further, wherein Sm (NO in the step 13)3Molar ratio with hexa is (2:1) ~ (1:2).
Further, packing ratio of the reaction precursor liquid in microwave hydrothermal liner is 50% in the step 2.
Further, in the step 2 under the conditions of 160 ~ 200 DEG C of microwave hydrothermals react 15 ~ 60min, reaction temperature and
Reaction time is to be determined that the higher the reaction time of temperature is relatively short according to the property and reaction condition of reactant, temperature compared with
Low the reaction time is appropriately extended, and full grown crystal can be obtained with this.
Further, the drying in the step 3 is dry 2 ~ 4h in 60 ~ 80 DEG C of electric vacunm drying case, dry
Too high or too low for temperature and drying time is too long or too short, cannot sufficiently dry and non-caking powder.
The invention has the advantages that the present invention is with Sm (NO3)3For samarium source, not only as alkali source but also made using hexa
For template, multilevel structure SmCO is carried out using microwave-hydrothermal method3(OH) preparation of crystallite.Obtained SmCO3(OH) crystallite
Purity is higher, and good crystallinity, oriented growth is obvious, and the flower-shaped multilevel structure that strip is self-assembled into is presented, and flower-shaped multilevel structure removes
Be conducive to outside the conduction of electronics, the absorbability of light is also promoted.SmCO is prepared relative to traditional hydro-thermal method3(OH),
The structure of product prepared by the present invention is 3D structure, and 3D structure is by zero dimension, one-dimensional and one of two-dimentional or a variety of basic
The composite material of structural unit composition, the 3D structure of same material are compared with other dimensions, because 3D structure has gathered other simultaneously
The advantage of dimension can show more excellent photoelectric characteristic；And preparation process is completed in a relatively short time.The reaction is with water
As reaction dissolvent, safety is good, and feasibility is strong, easy to operate, very economical, practical, has good industrial prospect.This
The conduction that the flower-shaped multilevel structure that strip obtained is self-assembled into is conducive to electronics is invented, so that SmCO3(OH) in solid-state electronic
It has great application prospect in component and superconductor.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is SmCO prepared by the present invention3(OH) X-ray diffraction (XRD) figure of crystallite.
Fig. 2 is SmCO prepared by the present invention3(OH) scanning electron microscope (SEM) figure of crystallite.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1:
Step 1 will analyze pure Sm (NO3)3·6H2O, which is dissolved in 50mL distilled water, is made Sm3+Concentration is 0.5molL-1's
Solution；
Step 2 will analyze pure hexa addition 0.5molL under magnetic stirring-1 Sm(NO3)3In solution,
So that Sm3+Molar ratio with hexa is 2:1, continues that 100mL microwave hydrothermal reaction liner is added after stirring 10min
In；Reaction precursor liquid is placed in microwave hydrothermal instrument, 170 DEG C of reaction 30min is warming up to, naturally cools to room after reaction
Temperature；
Step 3, product successively utilize distilled water and dehydrated alcohol centrifuge washing 4 times, are placed in 60 DEG C of electric vacunm drying
Dry 4 h in case, that is, obtain the bouquet that irregular sheet is self-assembled into, tightly packed between piece, and the size of bouquet is inhomogenous.
Embodiment 2:
Step 1 will analyze pure Sm (NO3)3·6H2O, which is dissolved in 50mL distilled water, is made Sm3+Concentration is 0.25molL-1
Solution；
Step 2 will analyze pure hexa addition 0.25molL under magnetic stirring-1 Sm(NO3)3In solution,
So that Sm3+Molar ratio with hexa is 1:1, continues that 100mL microwave hydrothermal reaction liner is added after stirring 10min
In；Reaction precursor liquid is placed in microwave hydrothermal instrument, 170 DEG C of reaction 45min is warming up to, naturally cools to room after reaction
Temperature；
Step 3, product successively utilize distilled water and dehydrated alcohol centrifuge washing 5 times, are placed in 70 DEG C of electric vacunm drying
The flower-shaped multilevel structure that dry 3 h in case, i.e. acquisition strip are self-assembled into, and good dispersion, size uniformity.
Embodiment 3:
Step 1 will analyze pure Sm (NO3)3·6H2O, which is dissolved in 50mL distilled water, is made Sm3+Concentration is 0.4molL-1's
Solution；
Step 2 will analyze pure hexa addition 0.4molL under magnetic stirring-1 Sm(NO3)3In solution,
So that Sm3+Molar ratio with hexa is 1.5:1, continues to be added in the reaction of 100mL microwave hydrothermal after stirring 10min
In lining；Reaction precursor liquid is placed in microwave hydrothermal instrument, 200 DEG C of reaction 15min is warming up to, naturally cools to room after reaction
Temperature；
Step 3, product successively utilize distilled water and dehydrated alcohol centrifuge washing 6 times, are placed in 80 DEG C of electric vacunm drying
Dry 2 h in case, that is, obtain the bouquet that irregular sheet is self-assembled into, tightly packed between piece, and the size of bouquet is inhomogenous.
Embodiment 4:
Step 1 will analyze pure Sm (NO3)3·6H2O, which is dissolved in 50mL distilled water, is made Sm3+Concentration is 0.35molL-1
Solution；
Step 2 will analyze pure hexa addition 0.35molL under magnetic stirring-1 Sm(NO3)3In solution,
So that Sm3+Molar ratio with hexa is 1:1.5, continues that 100mL microwave hydrothermal reaction liner is added after stirring 10min
In；Reaction precursor liquid is placed in microwave hydrothermal instrument, 180 DEG C of reaction 30min is warming up to, naturally cools to room after reaction
Temperature；
Step 3, product successively utilize distilled water and dehydrated alcohol centrifuge washing 4 times, are placed in 80 DEG C of electric vacunm drying
Dry 2 h in case, the i.e. product of the mixing pattern of acquisition strip and flower-like structure.
Embodiment 5:
Step 1 will analyze pure Sm (NO3)3·6H2O, which is dissolved in 50mL distilled water, is made Sm3+Concentration is 0.2molL-1's
Solution；
Step 2 will analyze pure hexa addition 0.2molL under magnetic stirring-1 Sm(NO3)3In solution,
So that Sm3+Molar ratio with hexa is 1:2, continues that 100mL microwave hydrothermal reaction liner is added after stirring 10min
In；Reaction precursor liquid is placed in microwave hydrothermal instrument, 160 DEG C of reaction 60min is warming up to, naturally cools to room after reaction
Temperature；
Step 3, product successively utilize distilled water and dehydrated alcohol centrifuge washing 4 times, are placed in 60 DEG C of electric vacunm drying
Dry 4 h in case, i.e. the acquisition non-uniform random plate cross structure of size.
Sm in embodiment 23+Proportion with the amount of hexa substance is 1:1, at this time six methylenes in reaction system
Urotropine hydrolyzes mostly is changed into OH-And CO3 2-, with the Sm to dissociate in solution3+In conjunction with being formed by monoclinic phase SmCO3(OH) brilliant
Core grows into elongate configuration in the two-dimensional direction, and three-dimensional flower-shaped knot is self-assembled under the action of intermolecular hydrogen bonding and Van der Waals force
Structure and good dispersion, size are more uniform.
Fig. 1 is SmCO prepared by the embodiment of the present invention 23(OH) XRD diagram of crystallite can obtain the product of preparation
No. JCPDS is 41-0663, as SmCO3(OH), from which further follow that purity is high, the crystallinity of product are strong, crystal structure is monocline
Phase, orientation growth are obvious.
Fig. 2 is SmCO prepared by the embodiment of the present invention 23(OH) scanned photograph that crystallite is shot when amplifying 10,000 times,
Product is the flower-like structure that strip is self-assembled into, good dispersion as seen from the figure.
For the present invention using hexa not only as alkali source but also as template, hexa is a kind of weak organic
Alkali, when temperature be higher than 150 DEG C, NH can be decomposed into through hydrolytic process4 +、OH-And CO3 2-, and there are four mutually for hexa tool
The structure feature of condensed Trianacyclohexane ring, is easily complexed with metal ion in liquid phase reaction course, and to product
Nucleation and crystalline growth process play certain regulating and controlling effect.
Many experiments discovery, the pattern of suitable samarium ion concentrations on product has a certain impact, when samarium ion concentration mistake
It cannot get three-dimensional multistage structure when small and excessive；The increase of hexa additional amount is so that OH in reaction system-With
CO3 2-Concentration increase, the nucleation amount of product increases, and a large amount of nucleus is in the state for growth of vying each other；In addition, reactant
The presence of excessive hexa in system can be also adsorbed on certain crystal faces of crystal grain, it is suppressed that difference is intercrystalline certainly
Assembling process, and finally obtained the production of the mixing pattern and random plate cross structure of part strip and flower-like structure
Object；As the additional amount for reducing hexa in reaction system, excessive Sm3+It is adsorbed on grain surface, is influenced in two-dimensional directional
Reach full growth, obtained more particle and the mixing pattern of flower-shaped multilevel structure that strip is self-assembled into.When reaction precursor liquid
PH=8 ~ 9, product can be generated, adjust the additional amount of hexa, be to regulate and control to product morphology.Replacement
Alkali source will be unable to obtain multilevel structure of the invention, and when using sodium carbonate and urea for alkali source, product is octahedral structure.
The present invention provides a kind of microwave-hydrothermal methods being simple and efficient to prepare multilevel structure SmCO3(OH) method of crystallite.
The reaction time of microwave-hydrothermal method is short, and instrument and equipment is simple, easy to operate, is easy to control；The present invention chooses hexa
Not only it had been used as alkali source but also had been used as template, and realized multilevel structure SmCO under specified conditions3(OH) controlledly synthesis of crystallite.
Each embodiment in this specification is all made of relevant mode and describes, same and similar portion between each embodiment
Dividing may refer to each other, and each embodiment focuses on the differences from other embodiments.Especially for system reality
For applying example, since it is substantially similar to the method embodiment, so being described relatively simple, related place is referring to embodiment of the method
Part explanation.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the scope of the present invention.It is all
Any modification, equivalent replacement, improvement and so within the spirit and principles in the present invention, are all contained in protection scope of the present invention
It is interior.
Claims (2)
1. monoclinic phase SmCO3(OH) preparation method of multilevel structure crystallite, which is characterized in that specifically follow the steps below:
Step 1, under agitation by hexa be added Sm (NO3)3In solution, continue before stirring 10min formation reaction
Drive liquid；
Reaction precursor liquid is placed in microwave hydrothermal liner and reacts by step 2, generates precipitating, naturally cools to room after reaction
Temperature；
Step 3 isolates the precipitating in step 2 and washs drying, obtains the flower-like structure SmCO that strip is self-assembled into3(OH) micro-
It is brilliant；
Wherein Sm (NO in the step 13)3Molar ratio with hexa is (2:1) ~ (1:2)；
Packing ratio of the reaction precursor liquid in microwave hydrothermal liner is 50% in the step 2；
15 ~ 60min is reacted in the step 2 under the conditions of 160 ~ 200 DEG C of microwave hydrothermals；
Sm (NO in the step 13)3The concentration of solution is 0.2 ~ 0.5molL-1, pH=8 ~ 9 of reaction precursor liquid.
2. monoclinic phase SmCO according to claim 13(OH) preparation method of multilevel structure crystallite, which is characterized in that described
Drying in step 3 is dry 2 ~ 4h in 60 ~ 80 DEG C of electric vacunm drying case.
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| CN105032392A (en) * | 2015-07-27 | 2015-11-11 | 陕西科技大学 | Method for preparing SmCO3 (OH)/ZnO nanocomposite by homogeneous hydrothermal method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105032392A (en) * | 2015-07-27 | 2015-11-11 | 陕西科技大学 | Method for preparing SmCO3 (OH)/ZnO nanocomposite by homogeneous hydrothermal method |
Non-Patent Citations (1)
| Title |
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| "Microwave-Assisted Hydrothermal Synthesis of Sm2O3 Nanoparticles and their Optical Properties";Hansong Xue et al.;《Journal of Nano Research》;20170310;第46卷;第100-110页 * |
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