CN108328644A - A kind of rodlike porous Er/Eu-ZnO composite material and preparation methods of rule - Google Patents
A kind of rodlike porous Er/Eu-ZnO composite material and preparation methods of rule Download PDFInfo
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- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
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Abstract
The present invention relates to a kind of rodlike porous Er/Eu ZnO composite material and preparation methods of rule, belong to technical field of nanometer material preparation.It is combined using template and hydro-thermal method, first uses CTAB for template, Zn (CH3COO)2For zinc source, prepare pure ordered porous zinc oxide precursor, the Europium chloride of different quality containing and erbium chloride are assembled into porous ZnO matrix using hydro-thermal method again, Europium chloride and erbium chloride are guest species and mineralizer, under hydrothermal conditions, induction obtains the rodlike porous Er/Eu ZnO composite materials of rule.Prepared composite material has regular duct and larger specific surface area, has very strong adsorption capacity to fluid.It is observed by scanning electron microscope, which has longer club shaped structure, and pattern rule is uniform, and the incorporation of rare earth ion promotes the transmitting of zno-based body, the material of this kind of novel nano structure will be with important application prospects in field of light emitting materials.The method of the present invention is simple and practicable, can be mass, has broad application prospects.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, and in particular to a kind of rodlike porous Er/Eu-ZnO of rule is compound
Material and preparation method thereof.
Background technology
Mesoporous material refers to aperture between 2-50nm and porosity is more than 40% ordered porous road material.According to
The size porous material in aperture can be divided into three kinds:Poromerics (microporous materials, d < 2nm), mesoporous material
(mesoporous materials, 2 < d < 50nm) and large pore material (macroporous materials, d>50nm).It is right
For porous nanometer material, after total pore volume (porosity) reaches certain value, if aperture is sufficiently small, it can also show and portal
Dimensional effect and skin effect, to generate a series of different properties with body phase.According to chemical composition come to mesoporous material into
Row classification, porous material can be divided into two big types of silicon substrate and non-silicon-based.Most study is exactly mesoporous material in silica-base material
Expect MCM series and SBA series;Non-silicon-based mesoporous material mainly includes oxide, sulfide and the phosphate etc. of transition metal.This
A little materials are generally possible to, there are a variety of variable valence states, have a wide range of applications.According to structure whether the mesoporous material of ordered pair
Material is classified, and two major class of orderly and unordered mesoporous material can be divided into.In terms of unordered mesoporous material, the magnitude range in aperture
It changes greatly, hole road shape comparatively very irregular.The duct regular shape of ordered mesoporous material, structural arrangement aspect are opposite
Orderly, and the size in aperture is relatively uniform, and can change experiment condition by mesoporous material certain size size model
It encloses interior continuously adjustable.Mesoporous material has a series of advantageous property:
(1) has well-regulated pore passage structure, the low angle direction on X ray diffracting spectrum there are strong Bragg diffraction maximums
In the presence of;(2) distribution in aperture is narrow, and the size in aperture is adjustable between 1.5-10nm;(3) there is different structures, hole wall (bone
Frame) composition, property and shape;(4) by the way that optimum conditions or by subsequent processing, there is good thermal stability and water
Thermal stability;(5) diversity of inorganic component;(6) high specific surface area, highest may be up to 1000m2/ g and high hole
Rate;(7) particle has irregular figure, the good duct order of height can be kept in micro-meter scale, and can control;
(8) in microstructure, the hole wall of mesoporous material is amorphous, and the orderly skeleton structure of this and micro porous molecular sieve has very big difference
Not, but it is not meant to that micropore is not present in hole wall;(9) orderly duct can be used as " microreactor ", and assembling wherein has and receives
Become " host-guest material " after uniform and stable " object " material of metrical scale, due to host and guest's bulk effect between its master, object
And guest materials small-size effect, the quantum size effect etc. that may have are allowed to be expected in electrode material, photoelectric device, micro-
The fields such as electronic technology, chemical sensor, nonlinear optical material are widely used;(10) there is the selection of preferable gas
Property and permeability.
The synthetic method of mesoporous material mainly has template, in situ synthesis, sol-gel method and hydro-thermal method etc..Template
Method is and a kind of most wide method using earliest, and specific template is added in preparation process, and so that material is had special
Pore passage structure.In field of nanometer material technology, templated synthesis is a kind of simple and effective method, can synthesize various nano materials, such as:
Metal, oxide, sulfide, polymer and various composite nano tubes, cable architecture.Hydro-thermal method poromerics is mostly first logical
It crosses other methods and prepares nanoparticle, the presomas such as nano wire or nanometer rods, then using it as matrix, coated on its surface,
Method to obtain compound particle.Hydro-thermal method by matrix and can be incorporated sundries and be assemblied together well, and often may be used
Pattern is special to obtain, the good nano material of isotypy, thus becomes a kind of important skill for the synthetic composite material receiving favor
Art.
Mesoporous zinc oxide is widely used in catalysis, gas sensor, liquid crystal display etc., with different preparations
Method, which produces mesoporous zinc oxide, can obtain the mesoporous material with different physicochemical properties, and wherein template plays important work
With.But the single mass of pure mesoporous zinc oxide cannot be satisfied the demand of people gradually, thus it is compound with mesoporous zinc oxide
The research for obtaining the more good composite material of property has greater significance.ZnO is a kind of relatively good ultraviolet absorption material, when
When ultraviolet lighting is mapped on sample surfaces, the lattice of the ZnO in composite material will soon absorb the purple as excitation light source
The energy of outer light, and store, then the energy by these storages passes to rare earth ion again, to excitation rare-earth ion
4f electronics makes it generate transition, further results in rare earth ion and generates red emission.So ZnO may be used as rare earth luminous material
The basis material of material, to improve the luminous efficiency of rare earth ion.The ionic radius of Li is very small, can be easier into ZnO's
In interstitial void, so LiOH is a kind of good sensitizer, the addition of LiOH can make rare earth ion more preferable, more effectively solid
It is molten and penetrate into the lattice dot matrix of zno-based body.Exactly because also in this way, in the preparation of composite material, Li+Play charge benefit
The effect repaid.There are one unique two-dimensional layered structures for ZnO crystal tool.In this way, cross-relaxation between rare earth ion can be by
It is limited on the adjacent node in the approximately the same plane in ZnO crystal.Due to Li+Ionic radius it is very small, in containing for preparation
Li+Composite material in, work as Li+When entering in the lattice dot matrix of ZnO, Li+Tend to enter the sun between layer and layer
In ion defects.At the same time, due to the presence of charge-compensation effects, Li+It is more likely to close to rear earth ions distribution, and shape
It is right at cation, to balance negative electrical charge.Li+Doping can hinder or limit the high level excitation state electronics for closing on rare earth ion
Cross-relaxation between lower level excitation state electronics or ground state electron.The presence of these factors can improve rare earth ion jump
The transition probability for moving process enhances the transition transmitting of the excitation state of electronics.Er/Eu-ZnO composite material early stages also have been reported,
It is primarily used to up-conversion luminescent material, fluorescent material etc.;Main preparation method has solwution method, fusion method, chemical precipitation method
Deng;The microscopic appearance of material includes nanometer rods, nano wire, nanometer sheet etc..Due to the outstanding feature and performance advantage of porous material,
In recent years, research in terms of in relation to porous structure ZnO is gradually got up more, the method for synthesizing porous structure also emerges one after another,
Including the hydro-thermal method of one of method during invention.With porous Er/Eu-ZnO composite materials there are also report,
Such as:Senapati et al. reports use zinc nitrate hexahydrate and one to be hydrated acetic acid europium in hexa as organic ligand,
Nanometer rods [S.Senapati, Red the emitting Eu of the rodlike meso-hole structures of Eu/ZnO grown under thermal and hydric environment:ZnO
nanorods for highly sensitive fluorescence intensity ratio based optical
thermometry,2016,5(5):1-11];Lang Jihui etc. by using sol-gel method, hydro-thermal method and chemical precipitation method,
The different rare earth of doping in semiconductor oxide zinc, to measure characteristic [the rear-earth-doped ZnO nanos of Lang Jihui of its luminescence generated by light
Optical Properties [D] the Jiangsu Universitys of structure, 2010.];Balakrishna et al. utilizes ZnO:Eu3+/Er3+/Yb3+Film
It is deposited on Si substrates by sol-gel spin coating technique.Have studied Yb3+Concentration is to membrane structure, granule-morphology and light
Learn performance influence [Balakrishna A, Pathak T K, Coetsee-Hugo E, et al.Synthesis,
structure and optical studies of ZnO:Eu3+,Er3+,Yb3+,thin films:Enhanced up-
conversion emission[J].Colloids&Surfaces A Physicochemical&Engineering
Aspects,2018.];Yang et al. is prepared for single doped-glass TeO- of several heterogeneities using melting quenching technology
10ZnO-10NaO.Have studied the influence of group pairs of density, molal volume, refractive index and phonon-side band spectra.[Yang Y,Chen
B,Wang C,et al.Investigation on structure and optical properties of Er,Eu
single-doped NaO–ZnO–BO–TeO glasses[J].Optical Materials,2009,31(2):445-450.]
Deng.
The correlative study and the present invention reported at present are essentially different.From the pattern of material, though there is part material
Material has club shaped structure, but mostly uneven, and size is smaller, does not find that this length of the present invention reaches 15-25 μm or so,
Width reaches the regular club shaped structure of 300-700nm, and the club shaped structure of material prepared by the present invention is received by ZnO one by one
Made of rice grain accumulation, particle surface is dispersed with orderly porous structure;From the synthetic method of material, using template
First synthesizing ordered porous ZnO as presoma is to obtain the antecedent basis of the rodlike porous material of this kind of rule to method, this research was once
It explores other rare earth ions and carries out structure directing, fail to obtain the material of the pattern, and in the presence of only Eu
The material morphology of the present invention can just be obtained;In view of luminescent properties, the addition of two kinds of rare earths of Eu/Er can enhance zinc oxide
In the intensity of 418nm transmittings.In addition, hydrothermal temperature, the parameters such as hydro-thermal time are groped again and again by us
It arrives.Although the material composition that the present invention obtains is similar with other correlative study, material morphology prepared by the present invention
Regular special, good properties, the preparation method of material is determined by prolonged careful parameter one by one of groping, so originally
There is novelty on invention product pattern, there is advance in properties of product, have originality in preparation method.Material is prepared to send out
Luminescent material field, which possesses, is extremely widely applied foreground.The material synthesis method that the present invention explores is that other patterns ZnO is compound
The synthesis of material preparation, other semi-conducting materials provides warning taken from the overturned card ahead.
Invention content
Since the nano material of Template synthesis has following significant advantage compared to the nano material that other methods synthesize:
(1) there is comparable flexibility;(2) experimental provision is simple, and operating condition is mild;(3) ruler of nano material can be accurately controlled
Very little, pattern and structure;(4) it can prevent nano material from agglomeration occurs;(5) it realizes nano material synthesis and is assembled into one
Change, while the stably dispersing sex chromosome mosaicism of nano material can be solved.Template is according to the characteristics of its template itself and confinement ability
Different can be divided into two kinds of hard template and soft template again.The general character of the two is to provide the reaction compartment of a limited size, area
It is not that the former provides static duct, substance can only enter from opening inside duct;And the latter provides and is in
The cavity of dynamic equilibrium, substance can penetrate cavity wall diffusion disengaging.Hydro-thermal method has in terms of synthesizing inorganic nanometer functional material
Following advantage:(1) it is substantially reduced reaction temperature;(2) synthesis and crystallization, the flow that product can be completed with single step are simple;
(3) product proportioning (4) can be controlled and prepare single phase material;(5) advantage of lower cost;(6) it is easy to get and is orientated, completely
Crystal;(7) in the crystal of growth, the ambiance that crystal growth is adjusted in (8) can be equably doped.
The present invention is to use template first, uses cetyl trimethylammonium bromide (CTAB) as template, zinc acetate
(Zn(CH3COO)2) it is used as zinc source, pure ordered porous zno-based body is prepared, which mainly wants controlling reaction temperature, reacts
Time, the pH value etc. of reaction system.Then, the pure ordered porous zinc oxide of the above step synthesis is as presoma, Europium chloride
(EuCl3) and erbium chloride (ErCl3) it is mineralizer, utilize hydro-thermal method composition rule bar-shaped ordered mesopore Er/Eu-ZnO composite woods
Material.The process is as follows:
The synthesis of pure ordered porous zno-based body:
(1) CTAB of precise 0.5-5.0g is dissolved in the water of 250-2500mL, and is stirred evenly at 80 DEG C;
(2) sodium hydroxide solution that 1.5-6.5mL 2mol/L are added continues to be stirred to uniformly;
(3) it is slowly added into 2.5-5.0g acetic acid dihydrate zinc stirring 1-5h;
(4) it is slowly added into lithium hydroxide, until solution is in slightly alkaline;
(5) mixture stirs 1-4h at 80 DEG C;
(6) mixed solution is filtered, filters out product;
(7) products therefrom will be filtered in electric drying oven with forced convection, dried for 24 hours under the conditions of 60 DEG C;
(8) powdered product is put into crucible, 500 DEG C in Muffle furnace, calcines 2-8h, heating rate is 1 DEG C/min;
(9) it is cooled to room temperature, obtains order mesoporous zinc oxide matrix.
The synthesis of regular bar-shaped ordered mesopore Er/Eu-ZnO composite materials:
(1) 0.07-0.70g Europium chlorides are weighed respectively, 0.17-1.70g erbium chlorides, 0.25-2.50g sulfosalicylic acids,
Appropriate amount of deionized water rear chamber is added in a clean beaker in the pure zinc oxide ordered mesoporous material matrix of the above-mentioned preparations of 0.4-4.0g
12-48h is stirred under the conditions of temperature;
(2) said mixture is fitted into ptfe autoclave, is taken after reacting 2-8h in 100-180 DEG C of baking oven
Go out, cooled to room temperature;
(3) obtained mixture is washed three times with absolute ethyl alcohol, filters out product;
(4) products therefrom will be filtered in electric drying oven with forced convection, dried for 24 hours under the conditions of 60 DEG C;
(5) product is taken out, the rodlike porous Er/Eu-ZnO composite materials of rule are obtained.
Description of the drawings
Fig. 1 is the XRD diffraction spectras of the rodlike porous Er/Eu-ZnO composite materials of rule;
Fig. 2 is the SEM photograph of the rodlike porous Er/Eu-ZnO composite materials of rule, which doubles as Figure of abstract;
Fig. 3 is the TEM photos of the rodlike porous Er/Eu-ZnO composite materials of rule;
Fig. 4 is the EDS power spectrums of the rodlike porous Er/Eu-ZnO composite materials of rule;
Fig. 5 is the emission spectrum of the rodlike porous Er/Eu-ZnO composite materials of rule.
Specific implementation mode
CTAB (cetyl trimethylammonium bromide) selected by the present invention, NaOH, Zn (CH3COO)2·2H2O,LiOH,
ErCl3,EuCl3,SSA(C7H6O6S·2H2O) it is commercially available analysis net product, the self-control of deionized water laboratory;Glass used
Instrument and equipment is common instrument and equipment in laboratory.
Embodiment:
The CTAB for weighing 1g is dissolved in the water of 480mL, and is persistently stirred evenly under the conditions of 80 DEG C, is added
The sodium hydroxide solution of 3.5mL2mol/L continues to be stirred to uniformly, and the acetic acid dihydrate zinc that 4.92g is then added continues to be stirred to
It is slowly added into lithium hydroxide after uniformly, until solution is in slightly alkaline, mixture stir under the conditions of 80 DEG C to mixing of obtaining after 2h
Solution filtering is closed, the product filtered out is dried under the conditions of 60 DEG C for 24 hours, then by the powdered product after drying in electric heating bellows
It is put into crucible, 500 DEG C in Muffle furnace, 4h is calcined, obtains the order mesoporous zinc oxide matrix of product.
Weigh 0.1417g Europium chlorides, 0.3408g erbium chlorides, 0.4558g sulfosalicylic acids and the above-mentioned preparations of 0.8000g
Order mesoporous zinc oxide in a clean beaker, persistently stir 48h at ambient temperature after appropriate amount of deionized water is added, then
Obtained mixture is injected in ptfe autoclave, 5h is reacted under the conditions of 150 DEG C in drying box, naturally cools to room
Obtained mixture is washed three times with absolute ethyl alcohol, filters out product by temperature, by filtering products therefrom in electric drying oven with forced convection
In, it is dry under the conditions of 60 DEG C to take out product for 24 hours, obtain the rodlike porous Er/Eu-ZnO composite materials of rule.
Prepare the X-ray diffraction analysis result of Er/Eu-ZnO composite materials as shown in Figure 1, by with standard card
(PDF#36-1451) it comparing, it may be determined that the principal crystalline phase for preparing material is the structure of hexagonal wurtzite phase oxidation zinc, meanwhile, occur
Sulfosalicylic acid europium, the characteristic diffraction peak of sulfosalicylic acid erbium and sulfosalicylic acid zinc;The Er/Eu-ZnO composite materials of preparation
Electron scanning micrograph as shown in Fig. 2, can be seen that from photo prepare material present a length be 15-25 μm, it is straight
Diameter is the regular club shaped structure of 300-700nm;Fig. 3 is the transmission electron microscope photo of the Er/Eu-ZnO composite materials prepared, from photo
It can be seen that preparing above the regular club shaped structure of material, there is many orderly ducts;That Fig. 4 is provided is the Er/ prepared
The EDS power spectrums of Eu-ZnO composite materials, occur O, Zn, Si in sample, Er, Eu, the signal peak of the elements such as C, and wherein C comes from
The appearance of conducting resinl, Si elemental signals peak is since in test process, caused by sample powder is dispersed on silicon chip, O and Zn come
From the mesoporous zinc oxide matrix for preparing material, Er and Eu are further proved, material from the rare earth element being doped into zinc oxide
In there are zinc oxide and micro Er and Eu elements to be doped into zno-based body;Fig. 5 is the Er/Eu-ZnO for preparing compound
The emission spectrum that material obtains under 360nm ultraviolet excitations, as can be seen that sample is in 418nm and 465nm from the spectrogram
There are two emission peaks in place, they can be attributed to the transmitting of transition generation of the ZnO conduction bands to valence band, it was demonstrated that rare earth element
Incorporation promotes shining for zno-based body.
Certainly, the invention may also have other embodiments, without deviating from the spirit and substance of the present invention, ripe
It knows those skilled in the art and makes various corresponding change and deformations, but these corresponding changes and change in accordance with the present invention
Shape should all belong to the protection domain of appended claims of the invention.
Claims (2)
1. a kind of rodlike porous Er/Eu-ZnO composite materials of rule, which is characterized in that it is powder structure to prepare material, material
Main component is ZnO and Er, and Eu, stereoscan photograph, which is shown, prepares material in regular Rod-like shape, and surface is dispersed with orderly
Mesopore orbit.
2. a kind of preparation method of the rodlike porous Er/Eu-ZnO composite materials of rule as described in claim 1, feature exist
In first using CTAB as template, Zn (CH3COO)2As zinc source, using the ordered porous ZnO powder matrix of Template synthesis, so
Afterwards, using the ordered porous ZnO of synthesis as presoma, Europium chloride and erbium chloride are mineralizer, rodlike using hydro-thermal method composition rule
Porous Er/Eu-ZnO composite materials, step are:
(1) synthesis of ordered porous ZnO precursor:
It is dissolved in the water of 250-2500mL with the CTAB of assay balance precise 0.5-5.0g, and is stirred evenly at 80 DEG C,
The sodium hydroxide solution that 1.5-6.5mL 2mol/L are added continues to be stirred to uniformly, is slowly added into 2.5-5.0g acetic acid dihydrate zinc
1-5h is stirred, is slowly added into lithium hydroxide, while testing pH, until solution is in slightly alkaline, mixture stirs 1-4h at 80 DEG C,
Mixed solution is filtered, product is filtered out, filtering products therefrom is dried in 60 DEG C of electric drying oven with forced convections for 24 hours, after drying
Powdered product be put into crucible, 500 DEG C in Muffle furnace, calcine 2-8h, heating rate be 1 DEG C/min, take out product, be situated between
Hole zinc oxide matrix;
(2) synthesis of the rodlike porous Er/Eu-ZnO composite materials of rule
On weighing 0.07-0.70g Europium chlorides, 0.17-1.70g erbium chlorides, 0.25-2.50g sulfosalicylic acids and 0.4-4.0g
The order mesoporous zinc oxide precursor of preparation is stated in a clean beaker, is added after appropriate amount of deionized water and continues at ambient temperature
12-48h is stirred, is then injected obtained mixture in ptfe autoclave, in drying box under the conditions of 100-180 DEG C
2-8h is reacted, obtained mixture is washed three times with absolute ethyl alcohol, filters out product by cooled to room temperature, by filtering gained
Product is dry under the conditions of 60 DEG C to take out product for 24 hours in electric drying oven with forced convection, and it is multiple to obtain the rodlike porous Er/Eu-ZnO of rule
Condensation material, the prepared rodlike porous Er/Eu-ZnO composite materials of rule are characterized by having larger specific surface area, relatively
Big aperture and regular pore passage structure, can load larger molecule or group, and zno-based body has ultraviolet light relatively strong
Absorbability, and the transmitting of rare earth ion can be promoted by the energy transmission of absorption to the centre of luminescence, be a kind of and effective
Inorganic rare earth matrices of composite material.
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CN112530712A (en) * | 2020-11-26 | 2021-03-19 | 吉林大学 | Composite electrode material, preparation method thereof and supercapacitor |
CN112530712B (en) * | 2020-11-26 | 2022-02-22 | 吉林大学 | Composite electrode material, preparation method thereof and supercapacitor |
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