CN106190125A - A kind of YPO4: Eu3+micron ball luminescent material and preparation method thereof - Google Patents
A kind of YPO4: Eu3+micron ball luminescent material and preparation method thereof Download PDFInfo
- Publication number
- CN106190125A CN106190125A CN201610529702.8A CN201610529702A CN106190125A CN 106190125 A CN106190125 A CN 106190125A CN 201610529702 A CN201610529702 A CN 201610529702A CN 106190125 A CN106190125 A CN 106190125A
- Authority
- CN
- China
- Prior art keywords
- ypo
- preparation
- luminescent
- luminescent material
- micron
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- 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
- C09K11/7795—Phosphates
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a kind of YPO4: Eu3+Micron ball luminescent material and preparation method thereof.YPO of the present invention4: Eu3+The chemical formula of micron ball luminescent material is YxEu1‑xPO4.Its preparation method is as rare earth source using corresponding rare earth nitrate, using organophosphorus ester as phosphorus source and chelating agent, first in water and alcohol mixed solution, stirring forms mixed solution, then above-mentioned mixed solution is transferred to carry out in hydrothermal reaction kettle hydro-thermal reaction, the reactant liquor of gained sequentially passes through filter, washs, is centrifuged, is dried, and finally gives a kind of YPO4: Eu3+Micron ball luminescent material.The YPO of the present invention4: Eu3+The preparation method reaction temperature of micron ball luminescent material is low, low for equipment requirements, operates fairly simple, the YPO obtained4: Eu3+Micron ball luminescent material morphology controllable, luminescent properties is good.
Description
Technical field
The invention belongs to rare earth luminescent material technical field, particularly relate to a kind of YPO4: Eu3+Micron ball luminescent material and
Preparation method.
Background technology
Yttrium phosphate belongs to tetragonal phase structure, is a kind of excellent host material, trivalent of can adulterating transition metal ion and
Rare earth ion synthesis has the luminescent material of different purposes, owing to RE phosphate shows good optical characteristics, so
Luminescence studies for RE phosphate begins to as far back as eighties of last century the sixties.At present, LaPO4: Ce3+, Tb3+Have become as
Commercial green-fluorescent powder for lamp.
It addition, yttrium phosphate (the chemical formula Y of trivalent europium ion dopingxEu1-xPO4) also it is a kind of important red fluorescence powder,
Report at present and use ammonium dihydrogen phosphate, diammonium phosphate and ammonium hydrogen phosphate etc. to synthesize Y as the source of phosphate radicalxEu1-xPO4Nanometer
Granule/nanometer rods luminescent material.But had no patent report by organophosphorus ester as the phosphorus source preparing yttrium phosphate substrate.Luminous material
The luminescent properties of material and its form have much relations, and spheroidal particle can improve its close heap, thus improves its luminosity.Its
Fluorescent material is coated with the requirement of screen technique also in the urgent need to the fluorescent material of synthesizing spherical.
The main method of synthesizing spherical luminescent material has complex coprecipitation, sol-gal process, spray pyrolysis at present
And hydro-thermal method etc..Above easily there is agglomeration in the luminous body of two kinds of method synthesis, and pattern granule is uneven.Spray pyrolysis
The luminescent material typically more uniform spherical morphology of ratio of preparation, has the advantages such as controlled particle size, particle narrowly distributing, this
Method is then widely used in the preparation of globe-type luminescence body.It addition, utilize hydro-thermal method under cryogenic, add surfactant
Effect under, it is possible to particle diameter and pattern are preferably controlled, it is thus achieved that there is the powder body material of well-crystallized, it is also possible to obtain nanometer
The micron ball luminous body of granulation mass bunch.
Summary of the invention
An object of the present invention be in order to synthesize a kind of luminous intensity higher there is the rare earth luminous of micron ball pattern
Material i.e. YPO4: Eu3+Micron ball luminescent material.
It is a further object of the present invention to provide above-mentioned a kind of YPO4: Eu3+The preparation method of micron ball luminescent material.
A kind of YPO that the present invention provides4: Eu3+The preparation method of micron ball luminescent material, specifically comprises the following steps that
(1), after Yttrium trinitrate and europium nitrate being mixed in a solvent, it is 8～10 with ammonia regulation pH, obtains mixed solution；
(2) in the mixed solution that step (1) obtains, add organophosphorus ester, with the pH value of ammonia regulation system 8～
Between 10, stirring mixing after static 2～3h, hydro-thermal reaction in hydrothermal reaction kettle；
(3), after hydro-thermal reaction terminates, filter, Cake Wash, be dried to obtain YPO4: Eu3+Micron ball luminescent material.
In the present invention, in step (1), the mol ratio of described Yttrium trinitrate and europium nitrate is 1.8:0.2～1.98:0.02.
In the present invention, the concentration of the ammonia in step (1), step (2) is 2～6mol/L.
In the present invention, in step (1), described solvent is water, or is the mixed solvent of water and ethanol.
In the present invention, the mol ratio of organophosphorus ester and Yttrium trinitrate is 2:1.98～16:1.8.
In the present invention, in step (2), organophosphorus ester is triethyl phosphate.
In the present invention, in step (2), hydrothermal temperature is 140～180 DEG C, and the hydro-thermal reaction time is 24～72h.
In the present invention, in step (3), successively with water, washing with alcohol filter cake.
The present invention also provides for a kind of YPO4: Eu3+Micron ball luminescent material.The present invention can be by regulating the ratio of second alcohol and water
Obtaining the material of different-shape, when increasing along with alcohol solvent volume, the granule assembling micron ball is become sheet from nano-particle
Shape granule, luminous intensity also has certain change.
Compared to the prior art, the beneficial effects of the present invention is:
The present invention adds triethyl phosphate in preparation process: both as reaction raw materials, serves as again organic complexing agent；Joint
Save reaction raw materials, decrease again error.Synthesize the red YPO of morphology controllable4: Eu3+Micron ball luminescent material, it is luminous
Intensity is along with the change generation significant change of pattern.
Further, a kind of YPO in the present invention4: Eu3+Micron ball luminescent material, by changing tricresyl phosphate second in preparation process
The ratio of the amount of ester and dehydrated alcohol and distilled water, can be with sized size, and therefore, this preparation method can be controlled effectively
The red YPO of system4: Eu3+The granular size of micron ball luminescent material and pattern.
Accompanying drawing explanation
Fig. 1, the gained chemical formula of embodiment 1,2,3,4,5,6 and 7 are Y0.95Eu0.05PO4Red YPO4: Eu3+Luminous micro-
The X-ray powder diffraction figure of rice material.
Fig. 2, the chemical formula of embodiment 1 gained are Y0.95Eu0.05PO4Red YPO4: Eu3+The scanning of luminescent micron material
Electronic Speculum figure.
Fig. 3, the chemical formula of embodiment 2 gained are Y0.95Eu0.05PO4Red YPO4: Eu3+The scanning of luminescent micron material
Electronic Speculum figure.
Fig. 4, the chemical formula of embodiment 3 gained are Y0.95Eu0.05PO4Red YPO4: Eu3+The scanning of luminescent micron material
Electronic Speculum figure.
Fig. 5, the chemical formula of embodiment 4 gained are Y0.95Eu0.05PO4Red YPO4: Eu3+The scanning of luminescent micron material
Electronic Speculum figure.
Fig. 6, the chemical formula of embodiment 5 gained are Y0.95Eu0.05PO4Red YPO4: Eu3+The scanning of luminescent micron material
Electronic Speculum figure.
Fig. 7, the chemical formula of embodiment 6 gained are Y0.95Eu0.05PO4Red YPO4: Eu3+The scanning of luminescent micron material
Electronic Speculum figure.
Fig. 8, the chemical formula of embodiment 7 gained are Y0.95Eu0.05PO4Red YPO4: Eu3+The scanning of luminescent micron material
Electronic Speculum figure.
Fig. 9, the chemical formula of embodiment 1,4,7 gained are Y0.95Eu0.05PO4Red YPO4: Eu3+Luminescent micron material
Exciting light spectrogram.
Figure 10, the chemical formula of embodiment 1,4,7 gained are Y0.95Eu0.05PO4Red YPO4: Eu3+Luminescent micron material
Emission spectrum figure.
Figure 11, the chemical formula of embodiment 1,8,9,10,11 gained are Y1-xEuxPO4(x=0.03,0.05,0.07,0.09,
0.11) red YPO4: Eu3+The emission spectrum figure of luminescent micron material.
Detailed description of the invention
Below by specific embodiment and combine accompanying drawing the present invention is expanded on further, but it is not limiting as the present invention.
Employing Holland PANatical x-ray powder diffraction instrument (CuK α radiates,) redness prepared by mensuration
YPO4: Eu3+The structure of micron ball luminescent material.
Use the red YPO prepared by HITACHI S-3400N scanning electron microscope mensuration4: Eu3+Micron ball luminescent material
Particle size and pattern.
Use the red YPO prepared by the test of HITACHI F-4600 fluorescence spectrophotometer4: Eu3+Micron ball luminescent material
Excitation and emission spectra.
Embodiment 1
A kind of red YPO4: Eu3+Micron ball luminescent material, its chemical formula YxEu1-xPO4, wherein x=0.05.
Above-mentioned a kind of red YPO4: Eu3+The preparation method of micron ball luminescent material, specifically includes following steps:
Yittrium oxide and europium oxide are joined in dilute nitric acid solution, stirs under heating condition and dissolve, be made into concentration respectively
It is yttrium nitrate solution and the europium nitrate solution of 0.02 ± 0.001mol/L of 0.2 ± 0.01mol/L；
Measure 9.50 ± 0.01ml Yttrium trinitrate and 5.00 ± 0.01ml europium nitrate solution in beaker, after being thoroughly mixed
Obtain mixed solution.
Above-mentioned solution is joined in 30ml ± 0.01ml distilled water, stir 1h, be 8 with 3mol/L ammonia regulation pH.
Continuously add triethyl phosphate 2mmol, again regulate pH value to 8 with 3mol/L ammonia, under room temperature, continue stirring 2h
After, proceed in the polytetrafluoroethyllining lining autoclave of 50ml, autoclave sealed, then react 40h at 170 DEG C of incubation water heatings,
Then the reactant liquor obtained is naturally cooled to room temperature in atmosphere.
The filter cake of gained will be cooled to after the reacting liquid filtering of room temperature successively with deionized water and absolute ethanol washing 3～4
Secondary, remove the NH that may remain in end product4 +, NO3 -, organic complex ion, the most in atmosphere control temperature be 60 DEG C do
Dry, i.e. obtaining chemical formula is Y0.95Eu0.05PO4Red YPO4: Eu3+Luminescent material.
This example gained YPO4: Eu3+The granule of luminescent micron material is scanned through S-3400N scanning electron microscope instrument, its
Result is shown in Fig. 2, and the micron ball that as can be seen from Figure 2 gained sample is piled up by nano-particle forms, the size size of ball
Uneven.
Embodiment 2
A kind of red YPO4: Eu3+Micron ball luminescent material, its chemical formula YxEu1-xPO4, wherein x=0.05.
Above-mentioned a kind of red YPO4: Eu3+The preparation method of luminescent micron material, specifically includes following steps:
Yittrium oxide and europium oxide are joined in dilute nitric acid solution, stirs under heating condition and dissolve, be made into concentration respectively
It is yttrium nitrate solution and the europium nitrate solution of 0.02 ± 0.001mol/L of 0.2 ± 0.01mol/L；
Measure 9.50 ± 0.01ml Yttrium trinitrate and 5.00 ± 0.01ml europium nitrate solution in beaker, after being thoroughly mixed
Obtain mixed solution.
Above-mentioned solution is joined in the mixed solvent of 25ml ± 0.01ml distilled water and 5ml ± 0.01ml dehydrated alcohol,
Stirring 1h, is 8 with 3mol/L ammonia regulation pH.
Continuously add triethyl phosphate 2mmol, again regulate pH value to 8 with 3mol/L ammonia, under room temperature, continue stirring 2h
After, proceed in the polytetrafluoroethyllining lining autoclave of 50ml, autoclave sealed, then react 40h at 170 DEG C of incubation water heatings,
Then the reactant liquor obtained is naturally cooled to room temperature in atmosphere.
The filter cake of gained will be cooled to after the reacting liquid filtering of room temperature successively with deionized water and absolute ethanol washing 3～4
Secondary, remove the NH that may remain in end product4 +, NO3 -, organic complex ion, the most in atmosphere control temperature be 60 DEG C do
Dry, i.e. obtaining chemical formula is Y0.95Eu0.05PO4Red YPO4: Eu3+Luminescent micron material.
This example gained YPO4: Eu3+The granule of luminescent micron material is scanned through S-3400N scanning electron microscope instrument, its
Result is shown in Fig. 3, and the set of balls that as can be seen from the figure gained sample has nanometer sheet to pile up becomes, and its granular size is about 5 μm.
Embodiment 3
A kind of red YPO4: Eu3+Luminescent micron material, its chemical formula YxEu1-xPO4, wherein x=0.05.
Above-mentioned a kind of red YPO4: Eu3+The preparation method of luminescent micron material, specifically includes following steps:
Yittrium oxide and europium oxide are joined in dilute nitric acid solution, stirs under heating condition and dissolve, be made into concentration respectively
It is yttrium nitrate solution and the europium nitrate solution of 0.02 ± 0.001mol/L of 0.2 ± 0.01mol/L；
Measure 9.50 ± 0.01ml Yttrium trinitrate and 5.00 ± 0.01ml europium nitrate solution in beaker, after being thoroughly mixed
Obtain mixed solution.
Above-mentioned solution is joined in the mixed solvent of 20ml ± 0.01ml distilled water and 10ml ± 0.01ml dehydrated alcohol,
Stirring 1h, is 8 with 3mol/L ammonia regulation pH.
Continuously add triethyl phosphate 2mmol, again regulate pH value to 8 with 3mol/L ammonia, under room temperature, continue stirring 2h
After, proceed in the polytetrafluoroethyllining lining autoclave of 50ml, autoclave sealed, then react 40h at 170 DEG C of incubation water heatings,
Then the reactant liquor obtained is naturally cooled to room temperature in atmosphere.
The filter cake of gained will be cooled to after the reacting liquid filtering of room temperature successively with deionized water and absolute ethanol washing 3～4
Secondary, remove the NH that may remain in end product4 +, NO3 -, organic complex ion, the most in atmosphere control temperature be 60 DEG C do
Dry, i.e. obtaining chemical formula is Y0.95Eu0.05PO4Red YPO4: Eu3+Luminescent micron material.
This example gained YPO4: Eu3+The granule of luminescent micron material is scanned through S-3400N scanning electron microscope instrument, its
Result is shown in Fig. 4, and the bouquet that as can be seen from the figure gained sample is piled up by loose nanometer sheet forms, and grain diameter is about 4 μm.
Embodiment 4
A kind of red YPO4: Eu3+Luminescent micron material, its chemical formula YxEu1-xPO4, wherein x=0.05.
Above-mentioned a kind of red YPO4: Eu3+The preparation method of luminescent micron material, specifically includes following steps:
Yittrium oxide and europium oxide are joined in dilute nitric acid solution, stirs under heating condition and dissolve, be made into concentration respectively
It is yttrium nitrate solution and the europium nitrate solution of 0.02 ± 0.001mol/L of 0.2 ± 0.01mol/L；
Measure 9.50 ± 0.01ml Yttrium trinitrate and 5.00 ± 0.01ml europium nitrate solution in beaker, after being thoroughly mixed
Obtain mixed solution.
Above-mentioned solution is joined in the mixed solvent of 15ml ± 0.01ml distilled water and 15ml ± 0.01ml dehydrated alcohol,
Stirring 1h, is 8 with 3mol/L ammonia regulation pH.
Continuously add triethyl phosphate 2mmol, again regulate pH value to 8 with 3mol/L ammonia, under room temperature, continue stirring 2h
After, proceed in the polytetrafluoroethyllining lining autoclave of 50ml, autoclave sealed, then react 40h at 170 DEG C of incubation water heatings,
Then the reactant liquor obtained is naturally cooled to room temperature in atmosphere.
The filter cake of gained will be cooled to after the reacting liquid filtering of room temperature successively with deionized water and absolute ethanol washing 3～4
Secondary, remove the NH that may remain in end product4 +, NO3 -, organic complex ion, the most in atmosphere control temperature be 60 DEG C do
Dry, i.e. obtaining chemical formula is Y0.95Eu0.05PO4Red YPO4: Eu3+Luminescent micron material.
This example gained YPO4: Eu3+The granule of luminescent micron material is scanned through S-3400N scanning electron microscope instrument, its
Result is shown in Fig. 5, and as can be seen from the figure gained sample is made up of the flower-shaped granule of various nanometer sheet arrangements, the surface of sheet
Adhere to some nano-particle.
Embodiment 5
A kind of red YPO4: Eu3+Luminescent micron material, its chemical formula YxEu1-xPO4, wherein x=0.05.
Above-mentioned a kind of red YPO4: Eu3+The preparation method of luminescent micron material, specifically includes following steps:
Yittrium oxide and europium oxide are joined in dilute nitric acid solution, stirs under heating condition and dissolve, be made into concentration respectively
It is yttrium nitrate solution and the europium nitrate solution of 0.02 ± 0.001mol/L of 0.2 ± 0.01mol/L；
Measure 9.50 ± 0.01ml Yttrium trinitrate and 5.00 ± 0.01ml europium nitrate solution in beaker, after being thoroughly mixed
Obtain mixed solution.
Above-mentioned solution is joined in the mixed solvent of 10ml ± 0.01ml distilled water and 20ml ± 0.01ml dehydrated alcohol,
Stirring 1h, is 8 with 3mol/L ammonia regulation pH.
Continuously add triethyl phosphate 2mmol, again regulate pH value to 8 with 3mol/L ammonia, under room temperature, continue stirring 2h
After, proceed in the polytetrafluoroethyllining lining autoclave of 50ml, autoclave sealed, then react 40h at 170 DEG C of incubation water heatings,
Then the reactant liquor obtained is naturally cooled to room temperature in atmosphere.
The filter cake of gained will be cooled to after the reacting liquid filtering of room temperature successively with deionized water and absolute ethanol washing 3～4
Secondary, remove the NH that may remain in end product4 +, NO3 -, organic complex ion, the most in atmosphere control temperature be 60 DEG C do
Dry, i.e. obtaining chemical formula is Y0.95Eu0.05PO4Red YPO4: Eu3+Luminescent micron material.
This example gained YPO4: Eu3+The granule of luminescent micron material is scanned through S-3400N scanning electron microscope instrument, its
Result is shown in Fig. 6, and the lamellar ball particle that as can be seen from the figure gained sample is piled up by nanometer sheet forms, and granular size is uneven, separately
Outward, compactness is piled up different.Pile up less about 4 μm of more loose bouquet size, pile up tighter bouquet granule and be about 5～10
μm。
Embodiment 6
A kind of red YPO4: Eu3+Luminescent micron material, its chemical formula YxEu1-xPO4, wherein x=0.05.
Above-mentioned a kind of red YPO4: Eu3+The preparation method of luminescent micron material, specifically includes following steps:
Yittrium oxide and europium oxide are joined in dilute nitric acid solution, stirs under heating condition and dissolve, be made into concentration respectively
It is yttrium nitrate solution and the europium nitrate solution of 0.02 ± 0.001mol/L of 0.2 ± 0.01mol/L；
Measure 9.50 ± 0.01ml Yttrium trinitrate and 5.00 ± 0.01ml europium nitrate solution in beaker, after being thoroughly mixed
Obtain mixed solution.
Above-mentioned solution is joined in the mixed solvent of 5ml ± 0.01ml distilled water and 25ml ± 0.01ml dehydrated alcohol,
Stirring 1h, is 8 with 3mol/L ammonia regulation pH.
Continuously add triethyl phosphate 2mmol, again regulate pH value to 8 with 3mol/L ammonia, under room temperature, continue stirring 2h
After, proceed in the polytetrafluoroethyllining lining autoclave of 50ml, autoclave sealed, then react 40h at 170 DEG C of incubation water heatings,
Then the reactant liquor obtained is naturally cooled to room temperature in atmosphere.
The filter cake of gained will be cooled to after the reacting liquid filtering of room temperature successively with deionized water and absolute ethanol washing 3～4
Secondary, remove the NH that may remain in end product4 +, NO3 -, organic complex ion, the most in atmosphere control temperature be 60 DEG C do
Dry, i.e. obtaining chemical formula is Y0.95Eu0.05PO4Red YPO4: Eu3+Luminescent micron material.
This example gained YPO4: Eu3+The granule of luminescent micron material is scanned through S-3400N scanning electron microscope instrument, its
Result is shown in Fig. 7, the lamellar ball particle composition that as can be seen from the figure gained sample nanometer sheet is piled up, and granular size ratio is more uniform,
And compactness is more consistent.The sample topography synthesized under the conditions of can speculating this mixed solvent is best.
Embodiment 7
A kind of red YPO4: Eu3+Luminescent micron material, its chemical formula YxEu1-xPO4, wherein x=0.05.
Above-mentioned a kind of red YPO4: Eu3+The preparation method of luminescent micron material, specifically includes following steps:
Yittrium oxide and europium oxide are joined in dilute nitric acid solution, stirs under heating condition and dissolve, be made into concentration respectively
It is yttrium nitrate solution and the europium nitrate solution of 0.02 ± 0.001mol/L of 0.2 ± 0.01mol/L；
Measure 9.50 ± 0.01ml Yttrium trinitrate and 5.00 ± 0.01ml europium nitrate solution in beaker, after being thoroughly mixed
Obtain mixed solution.
Above-mentioned solution is joined in the mixed solvent of 30ml ± 0.01ml dehydrated alcohol, stir 1h, use 3mol/L ammonia
Regulation pH is 8.
Continuously add triethyl phosphate 2mmol, again regulate pH value to 8 with 3mol/L ammonia, under room temperature, continue stirring 2h
After, proceed in the polytetrafluoroethyllining lining autoclave of 50ml, autoclave sealed, then react 40h at 170 DEG C of incubation water heatings,
Then the reactant liquor obtained is naturally cooled to room temperature in atmosphere.
The filter cake of gained will be cooled to after the reacting liquid filtering of room temperature successively with deionized water and absolute ethanol washing 3～4
Secondary, remove the NH that may remain in end product4 +, NO3 -, organic complex ion, the most in atmosphere control temperature be 60 DEG C do
Dry, i.e. obtaining chemical formula is Y0.95Eu0.05PO4Red YPO4: Eu3+Luminescent micron material.
This example gained redness YPO4: Eu3+The granule of luminescent micron material is swept through S-3400N scanning electron microscope instrument
Retouching, its result is shown in Fig. 8, and as can be seen from the figure gained sample is different with the sample topography that above mixed solvent synthesizes, and presents
Be the ganoid granule of irregular approximate sphericity.
Above-described embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6 and the change of embodiment 7 gained
Formula is Y0.95Eu0.05PO4Red YPO4: Eu3+Luminescent micron material is detected by PANatical x-ray powder diffraction instrument
(see Fig. 1), it can be seen that the structure of the product of synthesis is pure tetragonal phase structure (JCPDF No:11-0254)；
Using F-4600 (HITACHI) fluorescence spectrophotometer is Y to chemical formula obtained by the above embodiments 10.95Eu0.05PO4
Obtained by luminescent micron material, embodiment 4, chemical formula is Y0.95Eu0.05PO4Chemical formula obtained by luminescent micron material, embodiment 7
For Y0.95Eu0.05PO4The fluorescence property of luminescent micron material is tested respectively, and concrete outcome is shown in Fig. 9, Figure 10 respectively.Fig. 9 is
Embodiment 1, embodiment 4 and embodiment 7 gained chemical formula are Y0.95Eu0.05PO4Red YPO4: Eu3+Swashing of luminescent micron material
Luminous spectrogram；As can be seen from Figure 9 by the Y of embodiment 1 gained0.95Eu0.05PO4Red YPO4: Eu3+Luminescent micron material
Excitation peak is better than embodiment and the red YPO of embodiment 7 gained4: Eu3+Luminescent micron material.Figure 10 is embodiment 1, implements
Example 4 and embodiment 7 gained chemical formula are Y0.95Eu0.05PO4Red YPO4: Eu3+The emission spectrum figure of luminescent micron material；From
Figure 10 can be seen that by the Y implementing 1 gained0.95Eu0.05PO4Red YPO4: Eu3+Luminescent micron material has superior HONGGUANG
Emitting performance, and it is better than embodiment 4 and chemical formula that embodiment 7 prepares is Y0.95Eu0.05PO4Red YPO4: Eu3+Luminous micro-
Rice material, wherein the luminous intensity of embodiment 4 is minimum, and this is probably can quencher the sending out of its surface adsorption of granule of lamellar heap bunch
The foreign ion of light is more and causes.
Embodiment 8
A kind of red YPO4: Eu3+Luminescent micron material, its chemical formula YxEu1-xPO4, wherein x=0.03.
Above-mentioned a kind of red YPO4: Eu3+The preparation method of luminescent micron material, specifically includes following steps:
Yittrium oxide and europium oxide are joined in dilute nitric acid solution, stirs under heating condition and dissolve, be made into concentration respectively
It is yttrium nitrate solution and the europium nitrate solution of 0.02 ± 0.001mol/L of 0.2 ± 0.01mol/L；
Measure 9.70 ± 0.01ml Yttrium trinitrate and 3.00 ± 0.01ml europium nitrate solution in beaker, after being thoroughly mixed
Obtain mixed solution.
Above-mentioned solution is joined in 30ml ± 0.01ml distilled water, stir 1h, be 8 with 3mol/L ammonia regulation pH.
Continuously add triethyl phosphate 2mmol, again regulate pH value to 8 with 3mol/L ammonia, under room temperature, continue stirring 2h
After, proceed in the polytetrafluoroethyllining lining autoclave of 50ml, autoclave sealed, then react 40h at 170 DEG C of incubation water heatings,
Then the reactant liquor obtained is naturally cooled to room temperature in atmosphere.
The filter cake of gained will be cooled to after the reacting liquid filtering of room temperature successively with deionized water and absolute ethanol washing 3～4
Secondary, remove the NH that may remain in end product4 +, NO3 -, organic complex ion, the most in atmosphere control temperature be 60 DEG C do
Dry, i.e. obtaining chemical formula is Y0.97Eu0.03PO4Red YPO4: Eu3+Luminescent micron material.
Embodiment 9
A kind of red YPO4: Eu3+Luminescent micron material, its chemical formula YxEu1-xPO4, wherein x=0.07.
Above-mentioned a kind of red YPO4: Eu3+The preparation method of luminescent micron material, specifically includes following steps:
Yittrium oxide and europium oxide are joined in dilute nitric acid solution, stirs under heating condition and dissolve, be made into concentration respectively
It is yttrium nitrate solution and the europium nitrate solution of 0.02 ± 0.001mol/L of 0.2 ± 0.01mol/L；
Measure 9.30 ± 0.01ml Yttrium trinitrate and 7.00 ± 0.01ml europium nitrate solution in beaker, after being thoroughly mixed
Obtain mixed solution.
Above-mentioned solution is joined in 30ml ± 0.01ml distilled water, stir 1h, be 8 with 3mol/L ammonia regulation pH.
Continuously add triethyl phosphate 2mmol, again regulate pH value to 8 with 3mol/L ammonia, under room temperature, continue stirring 2h
After, proceed in the polytetrafluoroethyllining lining autoclave of 50ml, autoclave sealed, then react 40h at 170 DEG C of incubation water heatings,
Then the reactant liquor obtained is naturally cooled to room temperature in atmosphere.
The filter cake of gained will be cooled to after the reacting liquid filtering of room temperature successively with deionized water and absolute ethanol washing 3～4
Secondary, remove the NH that may remain in end product4 +, NO3 -, organic complex ion, the most in atmosphere control temperature be 60 DEG C do
Dry, i.e. obtaining chemical formula is Y0.93Eu0.07PO4Red YPO4: Eu3+Luminescent micron material.
Embodiment 10
A kind of red YPO4: Eu3+Luminescent micron material, its chemical formula YxEu1-xPO4, wherein x=0.09.
Above-mentioned a kind of red YPO4: Eu3+The preparation method of luminescent micron material, specifically includes following steps:
Yittrium oxide and europium oxide are joined in dilute nitric acid solution, stirs under heating condition and dissolve, be made into concentration respectively
It is yttrium nitrate solution and the europium nitrate solution of 0.02 ± 0.001mol/L of 0.2 ± 0.01mol/L；
Measure 9.10 ± 0.01ml Yttrium trinitrate and 9.00 ± 0.01ml europium nitrate solution in beaker, after being thoroughly mixed
Obtain mixed solution.
Above-mentioned solution is joined in 30ml ± 0.01ml distilled water, stir 1h, be 8 with 3mol/L ammonia regulation pH.
Continuously add triethyl phosphate 2mmol, again regulate pH value to 8 with 3mol/L ammonia, under room temperature, continue stirring 2h
After, proceed in the polytetrafluoroethyllining lining autoclave of 50ml, autoclave sealed, then react 40h at 170 DEG C of incubation water heatings,
Then the reactant liquor obtained is naturally cooled to room temperature in atmosphere.
The filter cake of gained will be cooled to after the reacting liquid filtering of room temperature successively with deionized water and absolute ethanol washing 3～4
Secondary, remove the NH that may remain in end product4 +, NO3 -, organic complex ion, the most in atmosphere control temperature be 60 DEG C do
Dry, i.e. obtaining chemical formula is Y0.91Eu0.09PO4Red YPO4: Eu3+Luminescent micron material.
Embodiment 11
A kind of red YPO4: Eu3+Luminescent micron material, its chemical formula YxEu1-xPO4, wherein x=0.11.
Above-mentioned a kind of red YPO4: Eu3+The preparation method of luminescent micron material, specifically includes following steps:
Yittrium oxide and europium oxide are joined in dilute nitric acid solution, stirs under heating condition and dissolve, be made into concentration respectively
It is yttrium nitrate solution and the europium nitrate solution of 0.02 ± 0.001mol/L of 0.2 ± 0.01mol/L；
Measure 8.9 ± 0.01ml Yttrium trinitrate and 11.00 ± 0.01ml europium nitrate solution in beaker, after being thoroughly mixed
Obtain mixed solution.
Above-mentioned solution is joined in 30ml ± 0.01ml distilled water, stir 1h, be 8 with 3mol/L ammonia regulation pH.
Continuously add triethyl phosphate 2mmol, again regulate pH value to 8 with 3mol/L ammonia, under room temperature, continue stirring 2h
After, proceed in the polytetrafluoroethyllining lining autoclave of 50ml, autoclave sealed, then react 40h at 170 DEG C of incubation water heatings,
Then the reactant liquor obtained is naturally cooled to room temperature in atmosphere.
The filter cake of gained will be cooled to after the reacting liquid filtering of room temperature successively with deionized water and absolute ethanol washing 3～4
Secondary, remove the NH that may remain in end product4 +, NO3 -, organic complex ion, the most in atmosphere control temperature be 60 DEG C do
Dry, i.e. obtaining chemical formula is Y0.89Eu0.11PO4Red YPO4: Eu3+Luminescent micron material.
We select the Eu of the experimental technique doping variable concentrations of the best embodiment 1 of luminous intensity3+, and it is luminous to characterize it
Performance.Figure 11 be the chemical formula of embodiment 1,8,9,10,11 gained be Y1-xEuxPO4(x=0.03,0.05,0.07,0.09,
0.11) red YPO4: Eu3+The emission spectrum figure of luminescent micron material.It can be seen that when x value is 0.03 to 0.05
Time, the luminous intensity of sample strengthens successively；And when x value is by 0.05 to 0.11, the luminous intensity of sample is to weaken successively
, therefore it may be speculated that the YPO prepared by this method4, the value of optimum doping concentration x is 0.05.Sample Y0.05Eu0.05PO4
Luminous intensity the strongest.
Foregoing is only the basic explanation under present inventive concept, and according to technical scheme made any etc.
Effect conversion, all should belong to protection scope of the present invention.
Claims (9)
1. a YPO4: Eu3+The preparation method of micron ball luminescent material, it is characterised in that specifically comprise the following steps that
(1), after Yttrium trinitrate and europium nitrate being mixed in a solvent, it is 8～10 with ammonia regulation pH, obtains mixed solution；
(2) in the mixed solution that step (1) obtains add organophosphorus ester, with the pH value of ammonia regulation system 8～10 it
Between, stirring mixing after static 2～3h, hydro-thermal reaction in hydrothermal reaction kettle；
(3), after hydro-thermal reaction terminates, filter, Cake Wash, be dried to obtain YPO4: Eu3+Micron ball luminescent material.
Rubbing of preparation method the most according to claim 1, it is characterised in that in step (1), described Yttrium trinitrate and europium nitrate
That ratio is 1.8:0.2～1.98:0.02.
Preparation method the most according to claim 1, it is characterised in that the concentration of the ammonia in step (1), step (2) is 2
～6mol/L.
Preparation method the most according to claim 1, it is characterised in that in step (1), described solvent is water, or is water
Mixed solvent with ethanol.
Preparation method the most according to claim 1, it is characterised in that the mol ratio of organophosphorus ester and Yttrium trinitrate is 2:
1.98～16:1.8.
The most according to claim 1 or 5, preparation method, it is characterised in that in step (2), organophosphorus ester is tricresyl phosphate
Ethyl ester.
Preparation method the most according to claim 1, it is characterised in that in step (2), hydrothermal temperature is 140～180
DEG C, the hydro-thermal reaction time is 24～72h.
Preparation method the most according to claim 1, it is characterised in that in step (3), successively with water, washing with alcohol filter cake.
9. the YPO obtained according to the preparation method one of claim 1-8 Suo Shu4: Eu3+Micron ball luminescent material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610529702.8A CN106190125A (en) | 2016-07-07 | 2016-07-07 | A kind of YPO4: Eu3+micron ball luminescent material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610529702.8A CN106190125A (en) | 2016-07-07 | 2016-07-07 | A kind of YPO4: Eu3+micron ball luminescent material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106190125A true CN106190125A (en) | 2016-12-07 |
Family
ID=57465787
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610529702.8A Pending CN106190125A (en) | 2016-07-07 | 2016-07-07 | A kind of YPO4: Eu3+micron ball luminescent material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106190125A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106744779A (en) * | 2017-01-11 | 2017-05-31 | 陕西科技大学 | Hollow ball-shape bismuth phosphate europium nanoparticles and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4991084A (en) * | 1973-01-06 | 1974-08-30 | ||
| US20100148658A1 (en) * | 2008-12-11 | 2010-06-17 | General Electric Company | Methods for preparation of nanocrystalline rare earth phosphates for lighting applications |
| CN101899306A (en) * | 2009-05-27 | 2010-12-01 | 中国科学院理化技术研究所 | Nanoparticles with core-shell structure and near-infrared fluorescence and preparation method thereof |
| CN102277167A (en) * | 2011-08-26 | 2011-12-14 | 昆明理工大学 | Europium ion-doped aluminum magnesium phosphate fluorescent powder and preparation method thereof |
| CN103059861A (en) * | 2013-01-23 | 2013-04-24 | 上海应用技术学院 | Red YVO4:Eu<3+> light emitting microballoon and preparation method thereof |
| CN103131417A (en) * | 2013-03-16 | 2013-06-05 | 青岛科技大学 | Eu doped YPO4 microballoon and preparation method thereof |
| CN103239756A (en) * | 2012-02-03 | 2013-08-14 | 佛山兰赛特生物科技有限公司 | Biological active microsphere and preparation method thereof |
| CN104893726A (en) * | 2015-05-27 | 2015-09-09 | 陕西科技大学 | Self-assembly Eu<3+> doping YPO4 microspheres and preparation method thereof |
-
2016
- 2016-07-07 CN CN201610529702.8A patent/CN106190125A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4991084A (en) * | 1973-01-06 | 1974-08-30 | ||
| US20100148658A1 (en) * | 2008-12-11 | 2010-06-17 | General Electric Company | Methods for preparation of nanocrystalline rare earth phosphates for lighting applications |
| CN101899306A (en) * | 2009-05-27 | 2010-12-01 | 中国科学院理化技术研究所 | Nanoparticles with core-shell structure and near-infrared fluorescence and preparation method thereof |
| CN102277167A (en) * | 2011-08-26 | 2011-12-14 | 昆明理工大学 | Europium ion-doped aluminum magnesium phosphate fluorescent powder and preparation method thereof |
| CN103239756A (en) * | 2012-02-03 | 2013-08-14 | 佛山兰赛特生物科技有限公司 | Biological active microsphere and preparation method thereof |
| CN103059861A (en) * | 2013-01-23 | 2013-04-24 | 上海应用技术学院 | Red YVO4:Eu<3+> light emitting microballoon and preparation method thereof |
| CN103131417A (en) * | 2013-03-16 | 2013-06-05 | 青岛科技大学 | Eu doped YPO4 microballoon and preparation method thereof |
| CN104893726A (en) * | 2015-05-27 | 2015-09-09 | 陕西科技大学 | Self-assembly Eu<3+> doping YPO4 microspheres and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 严俊鹏: "稀土掺杂钼、磷酸盐发光材料的可控合成及发光性能", 《中国优秀硕士学位论文全文数据库，工程科技Ⅰ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106744779A (en) * | 2017-01-11 | 2017-05-31 | 陕西科技大学 | Hollow ball-shape bismuth phosphate europium nanoparticles and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Xiao et al. | Synthesis and luminescence properties of YVO4: Eu3+ cobblestone-like microcrystalline phosphors obtained from the mixed solvent-thermal method | |
| CN1119384C (en) | Rare earth borate and its precursor, preparation processes and use of borate as lumcinophore | |
| Lin et al. | Sol–gel synthesis and photoluminescent characteristics of Eu3+-doped Gd2O3 nanophosphors | |
| Zhang et al. | The new red luminescent Sr3Al2O6: Eu2+ phosphor powders synthesized via sol–gel route by microwave-assisted | |
| JP3875027B2 (en) | Method for producing spherical zinc orthosilicate-based green light-emitting phosphor | |
| US20090140203A1 (en) | Rare earth nano phosphor and method of preparing the same | |
| Tian et al. | A novel approach for preparation of Sr3Al2O6: Eu2+, Dy3+ nanoparticles by sol–gel–microwave processing | |
| US6042747A (en) | Method of preparing high brightness, small particle red-emitting phosphor | |
| CN1149275C (en) | Prepn. of europium activated yttrium-gadolinium borate phosphor | |
| CN103275715B (en) | Preparation method of rare earth molybdate matrix red nanophosphor | |
| CN100588610C (en) | Synthesis method of nano-fluorescent powder mixed with europium yttrium phosphate-vanadate | |
| CN106190125A (en) | A kind of YPO4: Eu3+micron ball luminescent material and preparation method thereof | |
| CN108893115A (en) | A kind of preparation method of the spherical red fluorescence powder of La doped yttrium europium oxide | |
| CN105462589A (en) | Core-shell structured Fe3O4@GdVO4:Eu<3+> magnetic nanometer luminescent material and preparation method thereof | |
| CN103059861A (en) | Red YVO4:Eu<3+> light emitting microballoon and preparation method thereof | |
| Wu et al. | Uniform KCaY (PO 4) 2: Eu 3+ phosphors: sol–gel method, morphology and luminescence properties | |
| JP2018080215A (en) | Manufacturing method of phosphate fluophor | |
| Zhang et al. | Synthesis of Y2O3: Eu3+ phosphors by surface diffusion and their photoluminescence properties | |
| Lee et al. | Single-Step Synthesis of Cubic Y 2 O 3: Eu 3+ Nanophosphor by Flame Spray Pyrolysis | |
| CN103979513B (en) | A kind of cocoon-like TbPO with good luminous performance4powder body and preparation method thereof | |
| Shimomura et al. | Synthesis of Y (P, V) O4: Eu3+ red phosphor by spray pyrolysis without postheating | |
| Zhang et al. | Core/shell Y (OH) CO3: Eu3+/YBO3: Eu3+ phosphors with sphericity, submicrometre size and non-aggregation characteristics | |
| Linsheng et al. | Characterization and photoluminescence of Lu2O3-Eu3+ nano-phosphor prepared by modified solution combustion method | |
| CN105776331A (en) | Self sacrificing template synthesis method for preparation of rare earth vanadate with LRH as template | |
| Gao et al. | Uniform and Well-Dispersed LuBO3 Hollow Microspheres: Synthesis, Formation and Photoluminescence Properties |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161207 |