CN109734120A - A kind of flower-like microsphere structure Potassium Yttrium Tungstate material and preparation method thereof - Google Patents
A kind of flower-like microsphere structure Potassium Yttrium Tungstate material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to luminescent material technical fields, and in particular to a kind of flower-like microsphere structure Potassium Yttrium Tungstate material and preparation method thereof.The present invention prepares flower-like microsphere structure Potassium Yttrium Tungstate by hydro-thermal method cosurfactant, and addition surfactant changes interfacial tension, nanometer sheet is made to be self-assembled into flower-like microsphere structure.The flower-like microsphere structure Potassium Yttrium Tungstate of preparation has biggish specific surface area, and surface-active, adsorption ability, catalytic capability and luminous intensity etc. are enhanced, and can effectively improve the photoelectric functional of material；Preparation method simple process of the invention, low in cost, reproducible, convenient post-treatment do not need high temperature sintering, energy conservation and environmental protection.It can be used as luminescent material to be widely used in sending out the fields such as high definition display equipment, photocatalysis, the conversion of agricultural sunlight, photoelectric device and biological fluorescent labelling.
Description
Technical field
The invention belongs to luminescent material technical fields, and in particular to a kind of flower-like microsphere structure Potassium Yttrium Tungstate material and its system
Preparation Method.
Background technique
Rear-earth-doped alkaline earth answers tungstate crystal (AB (WO4)2(A is alkaline-earth metal, B=Re=Y, Gd, La, Lu, Yb etc.)
Be a kind of outstanding laser host material, there is high nonlinear refractive index, good mechanical and physical and chemical performance, crystal structure without
Sequence, rare earth ion and alkaline-earth metal ions position are not fixed, and rare earth ion absorption peak is wider, material transfer efficiency and laser output
The all more general tungstate crystal material of energy is high, while [WO in crystal4]2-The stronger covalent bonding effect of group W-O, so that glimmering
Optical concentration quenching effect weakens, and increases active ions doping concentration, is a kind of optical material of great prospect, in remote sensing, doctor
The wide range of areas such as treatment, scientific research and communication have potential application.
It is a kind of nearly ball of 201310245935.1 entitled micro-nano Potassium Yttrium Tungstates in Chinese invention patent application number
A kind of closely spherical Potassium Yttrium Tungstate particle and preparation method thereof is disclosed in the patent of shape particle and preparation method thereof, it is above-mentioned close spherical
Potassium Yttrium Tungstate particle has many shortcomings in practical applications, since nearly spherical Potassium Yttrium Tungstate particle surface is smooth, without hole
The special appearance of diameter, it is not ideal enough on improving the performances such as light, electricity, magnetic and the catalysis of Potassium Yttrium Tungstate, and nearly spherical wolframic acid
Yttrium k particle needs high temperature sintering during the preparation process, and energy consumption is high, preparation cost is high.
Summary of the invention
In view of this, the present invention provides a kind of flower-like microsphere structure Potassium Yttrium Tungstate material and preparation method thereof.The system
Preparation Method prepares flower-like microsphere structure Potassium Yttrium Tungstate using hydro-thermal method cosurfactant, and preparation method is simple, obtained
Material specific surface area with higher, while the surface-active of material, adsorption ability, catalytic capability and luminous intensity
It improves a lot.
To achieve the goals above, the preparation method of a kind of flower-like microsphere structure Potassium Yttrium Tungstate of the invention comprising with
Lower step:
(1) ruthenium ion solution is added drop-wise in tungstate ion solution and forms mixed solution, europium ion solution is added drop-wise to above-mentioned
In mixed solution, adjusting pH value is 7.5 ~ 8, is stirring evenly and then adding into a certain amount of surfactant, is stirred by ultrasonic and forerunner is made
Liquid solution；Tungstate ion in the precursor solution, ruthenium ion, europium ion molar ratio be 2:1:1；
(2) precursor solution obtained in step (1) is fitted into autoclave, precursor solution obtains white through hydro-thermal sealing thermal insulation
Color precipitating, hydrothermal temperature are 100 DEG C ~ 135 DEG C, and soaking time is 15h ~ 19h, and reaction kettle is naturally cooled to room after reaction
Temperature；
(3) flower-like microsphere structure Yttrium Tungstate will be obtained after white precipitate obtained in step (2) cleaning, centrifugation, drying, grinding
Potassium.As a further improvement of the present invention, the molar ratio of surfactant described in step (1) and tungstate ion is 1.4:1.
As a further improvement of the present invention, surfactant as described in step (1) is cetyl trimethyl bromination
Ammonium (CTAB) or neopelex (SDBS).
As a further improvement of the present invention, surfactant as described in step (1) is cetyl trimethyl bromination
The mixed liquor or neopelex of ammonium and ethyl alcohol, the proportionate relationship of the cetyl trimethylammonium bromide and ethyl alcohol
For 0.5-2g:5mL.
As a further improvement of the present invention, cleaning described in step (3) is after first being cleaned with deionized water again with third
The mixed liquor that ketone and volume fraction of ethanol are 1:1 cleans.
To achieve the goals above, the present invention provides a kind of flower-like microsphere structure that the preparation method that basis is for example above-mentioned obtains
Potassium Yttrium Tungstate material, the flower-like microsphere structure Potassium Yttrium Tungstate material is by sheet KY (WO4)2Composition, shape is flower ball-shaped, bouquet
For scale between 2~8.5 μm, specific surface area is 31.677 m2/g。
Compared with prior art, the beneficial effects of the present invention are: the present invention is prepared by hydro-thermal method cosurfactant
Flower-like microsphere structure Potassium Yttrium Tungstate, addition surfactant change interfacial tension, nanometer sheet self assembly are made to utilize surfactant
Ordered aggregation microenvironment is template auxiliary synthesis flower-like microsphere structure Potassium Yttrium Tungstate.The flower-like microsphere structure Potassium Yttrium Tungstate of preparation
With biggish specific surface area, surface-active, adsorption ability, catalytic capability and luminous intensity etc. are enhanced, energy
Effectively improve the photoelectric functional of material；Material prepared by the present invention has the features such as purity is high, good crystalline, monodispersity is good.This
The preparation method simple process of invention, low in cost, reproducible, convenient post-treatment do not need high temperature sintering, energy conservation and environmental protection.It can
It is widely used in sending out high definition display equipment, photocatalysis, the conversion of agricultural sunlight, photoelectric device and bioluminescence as luminescent material
The fields such as label.
Detailed description of the invention
Fig. 1 is the scanning electron microscope diagram of flower-like microsphere structure Potassium Yttrium Tungstate prepared by embodiment 1；
Fig. 2 is the scanning electron microscope diagram of flower-like microsphere structure Potassium Yttrium Tungstate prepared by embodiment 2；
Fig. 3 is the scanning electron microscope diagram of flower-like microsphere structure Potassium Yttrium Tungstate prepared by embodiment 3；
Fig. 4 is the scanning electron microscope diagram of flower-like microsphere structure Potassium Yttrium Tungstate prepared by embodiment 4；
Fig. 5 is the scanning electron microscope diagram of flower-like microsphere structure Potassium Yttrium Tungstate prepared by embodiment 5；
Fig. 6 is the X-ray diffraction analysis figure of flower-like microsphere structure Potassium Yttrium Tungstate prepared by embodiment 5 and pair of standard PDF card
Than figure；
Fig. 7 is the adsorption desorption curve graph of flower-like microsphere structure Potassium Yttrium Tungstate prepared by embodiment 5；
Fig. 8 is launching light spectrogram of the flower-like microsphere structure Potassium Yttrium Tungstate of the preparation of embodiment 5 under 464nm excitation.
Specific embodiment
In order to which those skilled in the art better understood when technical solution provided by the present invention, below with reference to specific
Embodiment is illustrated.
Embodiment 1:
Weigh the K of 8mmol2WO4, 2.2mmol Y (NO3)3·6H2O is dissolved in deionized water respectively, is configured to 0.16mol/L
WO4 2-The Y of solution and 0.044mol/L3+Solion, by Y3+Solion is added drop-wise to WO dropwise4 2-In solution, after mixing
Stir 10min.Weigh the Eu (NO of 1.8mmol3)3It is dissolved in deionized water, is configured to the Eu of 0.036mol/L3+Solution, then by
It is added drop-wise in above-mentioned mixed solution, stirs 10min.Adjusting mixed liquor pH value again is 7.8, after by 0.5g 1.37m mol 16
Alkyl trimethyl ammonium bromide is (with K2WO4The ratio of amount of substance be 1:6) and the mixing of 5ml ethyl alcohol after be added in mixed liquor,
1h is stirred on magnetic stirring apparatus, and precursor solution is made.Precursor solution obtained is stood to heat preservation in 130 DEG C of water heating kettle
18 hours, the solution kept the temperature through hydro-thermal is filtered, clean filtrate, grinding obtains flower-like microsphere structure Potassium Yttrium Tungstate after drying.
As shown in Figure 1, microballoon size is at 8.1 μm or so.
Embodiment 2:
Weigh the K of 8mmol2WO4, 1.8mmol Y (NO3)3·6H2O is dissolved in deionized water respectively, is configured to 0.16mol/L
WO4 2-The Y of solution and 0.036mol/L3+Solion, by Y3+Solion is added drop-wise to WO dropwise4 2-In solution, stirred after mixing
Mix 10min.Weigh the Eu (NO of 2.2mmol3)3It is dissolved in deionized water, is configured to the Eu of 0.044mol/L3+Solution, then dropwise
It is added drop-wise in above-mentioned mixed solution, stirs 10min.Adjusting mixed liquor pH value again is 8, after by 2.74 mmol cetyl three of 1g
Methyl bromide ammonium is (with K2WO4The ratio of amount of substance be 1:3) and the mixing of 5ml ethyl alcohol after be added in mixed liquor, stirred in magnetic force
It mixes and stirs 1h on device, precursor solution is made.It is small that precursor solution obtained is stood to heat preservation 16 in 100 DEG C of water heating kettle
When, the solution kept the temperature through hydro-thermal is filtered, filtrate is cleaned, grinding obtains flower-like microsphere structure Potassium Yttrium Tungstate after drying.Such as Fig. 2
Shown, microballoon size is at 4.4 μm or so.
Embodiment 3:
Weigh the K of 8mmol2WO4It is dissolved in the WO that 0.16mol/L is configured in deionized water4 2-Solution weighs the Y of 1.5mmol2O3
It is dissolved in dust technology, is configured to the Y (NO of 0.06mol/L3)3Solution, by Y (NO3)3Solution is added drop-wise to WO dropwise4 2-In solution,
10min is stirred after mixing.Weigh the Eu of 0.5mmol2O3It is dissolved in dust technology, is configured to the Eu of 0.02mol/L3+Solution, then by
It is added drop-wise in above-mentioned mixed solution, stirs 10min.Adjusting mixed liquor pH value again is 7.2, after by 0.172 mmol ten of 0.06g
Dialkyl benzene sulfonic acids sodium is (with K2WO4The ratio of amount of substance be 1:47) be added in mixed liquor, stirred on magnetic stirring apparatus
Precursor solution is made in 1h.Precursor solution obtained is stood to heat preservation 19 hours in 100 DEG C of water heating kettle, it will be through hydro-thermal
The solution of heat preservation filters, and cleans filtrate, and grinding obtains flower-like microsphere structure Potassium Yttrium Tungstate after drying.As shown in figure 3, microballoon is big
It is small at 3.2 μm or so.
Embodiment 4:
The K of 4mmol is weighed respectively2WO4With the Y (NO of 1.7mmol3)3·6H2O, which is dissolved in deionized water, is configured to 0.08mol/L
WO4 2-The Y of solution and 0.034mol/L3+Solion, by Y3+Solion is added drop-wise to WO dropwise4 2-In solution, stirred after mixing
Mix 10min.Weigh the Eu of 0.075mmol2O3It is dissolved in dust technology, is configured to the Eu of 0.003mol/L3+Solution is added drop-wise to dropwise
In above-mentioned mixed solution, 10min is stirred；Adjusting mixed liquor pH value is 7.5, after by 2g 5.49mmol cetyl trimethyl bromine
Change ammonium (with K2WO4The ratio of amount of substance be 1.4:1) and 5ml ethyl alcohol be added in mixed liquor after mixing, stirred in magnetic force
It mixes and stirs 1h on device, precursor solution is made.It is small that precursor solution obtained is stood to heat preservation 19 in 120 DEG C of water heating kettle
When, the solution kept the temperature through hydro-thermal is filtered, filtrate is cleaned, grinding obtains flower-like microsphere structure Potassium Yttrium Tungstate after drying.Such as Fig. 4
Shown, microballoon size is at 5.7 μm or so.
Embodiment 5:
The K of 4mmol is weighed respectively2WO4With the Y (NO of 2mmol3)3·6H2O, which is dissolved in deionized water, is configured to 0.08mol/L's
WO4 2-The Y of solution and 0.04mol/L3+Solion, by Y3+Solion is added drop-wise to WO dropwise4 2-In solution, stirred after mixing
10min.Weigh the Eu of 0.075mmol2O3It is dissolved in dust technology, is configured to the Eu3+ solution of 0.003mol/L, is added drop-wise to dropwise
It states in mixed solution, stirs 10min；Adjusting mixed liquor pH value is 8, after by 5.49 mmol cetyl trimethylammonium bromide of 2g
(with K2WO4The ratio of amount of substance be 1.4:1) and 5ml ethyl alcohol be added in mixed liquor after mixing, in magnetic stirring apparatus
Precursor solution is made in upper stirring 1h.Precursor solution obtained is stood to heat preservation 19 hours in 100 DEG C of water heating kettle, it will
Solution filtering through hydro-thermal heat preservation, cleans filtrate, grinding obtains flower-like microsphere structure Potassium Yttrium Tungstate after drying.As shown in figure 5,
Microballoon size is at 2.3 μm or so.
By the flower-like microsphere structure Potassium Yttrium Tungstate material being prepared carry out X-ray diffraction analysis and with standard PDF card
It compares, as shown in fig. 6, all diffraction maximum crystal faces all correspond to monoclinic system KY (WO4)2Diffraction (the PDF NO of each crystal face
45-0472), occur without other impurity peaks, illustrate that preparing product is determined as Potassium Yttrium Tungstate.
The flower-like microsphere structure Potassium Yttrium Tungstate material being prepared is subjected to the test of isothermal nitrogen adsorption desorption, Fig. 7 is flower-shaped
The adsorption desorption curve graph of micro-sphere structure Potassium Yttrium Tungstate, wherein abscissa is relative pressure P/P0, ordinate is adsorptive value cm3/g；
As shown in fig. 7, the adsorption desorption curve type of sample is weak interaction, the specific surface area of sample is calculated according to BET formula
For 31.677 m2/g。
The flower-like microsphere structure Potassium Yttrium Tungstate being prepared is subjected to fluorometric investigation under 464nm exciting light, is emitted
Spectrum；Fig. 8 is launching light spectrogram of the flower-like microsphere structure Potassium Yttrium Tungstate under 464nm excitation；Wherein, abscissa is wavelength nm,
Ordinate is intensity a.u.；As shown in figure 8, spectrum line is mainly by between 500nm to 750nm under 464nm excitation wavelength
Peak composition.Respectively correspond Eu3+Ion5D0→7F1 (596nm) transition, is converted to sodium yellow；5D0→7F2(614nm) transition,
It is converted to orange-colored light, and emissive porwer is very big；5D0→7F4(704nm) transition, is converted to red light.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (6)
1. a kind of preparation method of flower-like microsphere structure Potassium Yttrium Tungstate, which comprises the following steps:
(1) ruthenium ion solution is added drop-wise in tungstate ion solution and forms mixed solution, europium ion solution is added drop-wise to above-mentioned
In mixed solution, adjusting pH value is 7.5 ~ 8, is stirring evenly and then adding into a certain amount of surfactant, is stirred by ultrasonic and forerunner is made
Liquid solution；Tungstate ion in the precursor solution, ruthenium ion, europium ion molar ratio be 2:1:1；
(2) precursor solution obtained in step (1) is fitted into autoclave, precursor solution hydro-thermal sealing thermal insulation obtains white
Precipitating, the hydrothermal temperature are 100 DEG C ~ 135 DEG C, and soaking time is 15h ~ 19h, after reaction naturally cools to reaction kettle
Room temperature；
(3) flower-like microsphere structure Yttrium Tungstate will be obtained after white precipitate obtained in step (2) cleaning, centrifugation, drying, grinding
Potassium.
2. the preparation method of flower-like microsphere structure Potassium Yttrium Tungstate according to claim 1, which is characterized in that in step (1)
The molar ratio of the surfactant and tungstate ion is 1.4:1.
3. the preparation method of flower-like microsphere structure Potassium Yttrium Tungstate according to claim 1, which is characterized in that in step (1)
The surfactant is cetyl trimethylammonium bromide or neopelex.
4. the preparation method of flower-like microsphere structure Potassium Yttrium Tungstate according to claim 1, which is characterized in that in step (1)
The surfactant is the mixed liquor of cetyl trimethylammonium bromide and ethyl alcohol, cetyl trimethylammonium bromide and second
The usage ratio relationship of alcohol is 0.5-2g:5mL.
5. the preparation method of flower-like microsphere structure Potassium Yttrium Tungstate according to claim 1, which is characterized in that in step (3)
The cleaning is to be cleaned again with the mixed liquor that acetone and volume fraction of ethanol are 1:1 after first being cleaned with deionized water.
6. a kind of flower-like microsphere structure Potassium Yttrium Tungstate material that preparation methods described in any item according to claim 1 ~ 5 obtain,
It is characterized in that, the flower-like microsphere structure Potassium Yttrium Tungstate material is by sheet KY (WO4)2Composition, shape is flower ball-shaped, bouquet ruler
For degree between 2~8.5 μm, specific surface area is 31.677 m2/g。
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| CN110759381A (en) * | 2019-11-05 | 2020-02-07 | 北华航天工业学院 | Preparation method of coral-shaped lithium vanadate nano material |
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