CN105694880B - A kind of fluorescent RE powder magnesium Indium phosphate host material and preparation method thereof - Google Patents
A kind of fluorescent RE powder magnesium Indium phosphate host material and preparation method thereof Download PDFInfo
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- CN105694880B CN105694880B CN201610235386.3A CN201610235386A CN105694880B CN 105694880 B CN105694880 B CN 105694880B CN 201610235386 A CN201610235386 A CN 201610235386A CN 105694880 B CN105694880 B CN 105694880B
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- 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
- C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
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- 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
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7737—Phosphates
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- 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
- C09K11/7743—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing terbium
- C09K11/7752—Phosphates
Abstract
A kind of fluorescent RE powder magnesium Indium phosphate host material and preparation method thereof, its chemical composition is Mg21‑28In28‑34P42‑48Oy(y=168 199).The preparation method is prepared from using wet-chemical solid sintering technology.Successfully research and development of the invention obtain it is a kind of it is new can as phosphor host phosphate compounds, wherein contain phosphide element, rare earth element can partly substitute phosphide element as Validation Counter and enter in parent lattice, thus the compound that the present invention is prepared can be as fluorescent material host material；There is not been reported for obtained this magnesium Indium phosphate host material of the invention in the prior art.The technique of the present invention has the features such as preparation technology is simpler.
Description
Technical field：
The present invention relates to rare earth luminescent material field, more particularly, to a kind of fluorescent RE powder magnesium Indium phosphate matrix material
Material and preparation method thereof.
Background technology：
In information age today, fluorescent material is widely used in illuminating, shows, decorates, detecting, the numerous areas such as false proof,
Turn into material indispensable in people's daily life.It is used as the important component of fluorescent material, performance of the matrix to product
Important, different matrix are because of its crystal structure difference, because residing crystalline field environment is different after active ions doping,
Engery level cracking situation difference, macroscopically shows as the difference of spectral quality.Phosphate is moderate because of its phonon energy, in vacuum
Ultraviolet-ultraviolet region has compared with strong absorption band, and the solubility to rare earth ion is high, and with physical and chemical performance stabilization, raw material
It is with low cost, be a kind of important phosphor host, with very high application value the advantages of preparation technology is simple.From
Since the seventies of last century six, the exploration using phosphate as the fluorescent material of matrix is also constantly carried out both at home and abroad, has been prepared for
A series of RE phosphate fluorescent material (LaPO available for different field4:Ce3+,Tb3+、(Sr,Mg)2P2O7:Eu2+), and show
Good optical property is gone out.From the point of view of anion structure, wherein research more application is wider mainly around orthophosphates
(PO4)nWith pyrophosphate (P2O7)nSeries, its matrix does not light in itself, but has in VUV-near ultraviolet band a stronger absorption,
This charge migration just between rare earth ion-coordination oxygen matches, and can effectively transfer energy to the centre of luminescence, and with
The form of light is radiated.Research work is surrounded based on the doping vario-property for having been reported compound mostly in the current field
And deploy, or a series of isostructural compoundses compared with mature substrate are studied, and explore the work of New-type matrix material then
It is relatively rare.A kind of noval chemical compound is from synthesis pure sample is found to, and its composition proportion etc. is all needed to explore by many experiments and determined；Separately
Outside, and not all compound is suitable as fluorescent material host material, it is desirable to which it has good heat endurance, and (fluorescent material exists
Room temperature long-time performance used above does not change) and chemical stability (fluorescent material is not decomposed or is not easy to react with device), purple
Outskirt has the characteristics such as absorption visible region high transmission, thus those skilled in the art are generally acknowledged that the mistake for exploring new host material
Journey is very difficult.
The content of the invention：
The purpose of the present invention aims to provide a kind of new fluorescent RE powder magnesium Indium phosphate host material.
Another object of the present invention is to there is provided the simple its preparation process of above-mentioned material.
The magnesium Indium phosphate matrix components expression formula Mg of the present invention21-28In28-34P42-48Oy, it is RE phosphate fluorescent material
Matrix, wherein y be molal quantity, y=168~199.
Described magnesium Indium phosphate host crystal belongs to anorthic system, P-1 (No.2) space group.
The magnesium Indium phosphate host material process that the present invention is synthesized is, according to Mg:In:P mol ratios are (21~28):(28
~34):(42~48), can weigh raw material MgO, In2O3And NH4H2PO4, and according to wet-chemical-synthesis in solid state legal system of the present invention
Standby technique, can obtain Mg21-28In28-34P42-48Oy(y=168~199) fluorescent material phosphate base material.
Polycrystal synthesis is carried out using wet-chemical-solid-phase sintering method in host material of the present invention, detailed process is such as
Under：Because the phosphor host is a kind of without report and the unknown new compound of structure, anti-using wet-chemical-solid phase
When induction method prepares fluorescent material sample, by Mg:In:P mol ratio is (21~28):(28~34):(42~48) weigh suitable
MgO, In of amount2O3And NH4H2PO4It is put into beaker, adds strong acid (such as nitric acid), heating stirring makes dissolution of raw material, treats that solution is clear
Add polyvinyl alcohol and deionized water (can also be the high water quality of other chemical purities) after clear, heating stirring to being evaporated completely,
The grinding of dried material is uniform；First stage sintering is carried out at 1100-1300 DEG C, room temperature is cooled to, ground, Ran Hou
Second stage sintering is carried out under 1100-1300 DEG C of temperature conditionss, is cooled down, grinding obtains final product.
The heating rate of first stage sintering step is preferably 3~7 DEG C/min in preparation process of the present invention.
The heating rate of second stage sintering step is preferably 3~7 DEG C/min in preparation process of the present invention.
The soaking time of first stage sintering step is preferably 10~20 hours in preparation process of the present invention.
The soaking time of second stage sintering step is preferably 10~20 hours in preparation process of the present invention.
Because the phosphor host of the present invention is to be a kind of without reporting the compound with new crystal structure, invention
People has found that the ideal linearity molecular formula of the matrix is Mg by studying3In4P6O24, because Mg/In/P mutually has one in lattice
Determine solid solubility, its actual solid solution molecular formula is Mg21-28In28-34P42-48Oy(y=168-199).Utilize the matrix material of the present invention
The X-ray powder diffraction data of material, using Fullprof softwares carry out indexing, show that the material belongs to anorthic system, P-1
(No.2) space group.Inventor by host material of the present invention by comparing joint committee (ICDD) powder diffraction
Database (PDF-4+2011) and Inorganic crystal structure database (ICSD) and the softwares of MDI jade 5.0, it may be determined that the present invention
The matrix is a kind of crystal structure new compound that there is not been reported.
Beneficial effects of the present invention
The present invention first successfully research and development obtain it is a kind of it is new can as phosphor host phosphate chemical combination
Thing, wherein containing phosphide element, rare earth element can partly substitute phosphide element as Validation Counter and enter in parent lattice, thus this hair
The bright compound prepared can be used as fluorescent material host material；Obtained this magnesium indium phosphorus of the invention in the prior art
There is not been reported for hydrochlorate host material.The technique of the present invention has the features such as preparation technology is simpler.
Brief description of the drawings：
Fig. 1 is embodiment 1, and comparative example 1-3 XRD spectrum compares；
In Fig. 1 it is unmarked go out diffraction maximum correspondence the present invention Mg21-28In28-34P42-48OyDiffraction maximum.Can from figure
Go out, embodiment 1, contain Mg in the sample XRD spectrum obtained by comparative example 1-321-28In28-34P42-48OyDiffraction maximum, comparative example
Product made from 1~comparative example 3 is mixed phase, and the product obtained by embodiment 1 is Mg in the present invention21-28In28-34P42-48Oy
The single phase composition sample of phosphor host.
Fig. 2 is embodiment 1, embodiment 2, the XRD spectrum of 3 three samples of embodiment compare；
It can be seen that sample XRD spectrum made from embodiment 2, embodiment 3 and the sample XRD spectrum of embodiment 1 are complete
It is complete consistent, occur without miscellaneous peak, be Mg in the present invention21-28In28-34P42-48OyThe single phase composition sample of phosphor host
Product.
Fig. 3 is embodiment 1, and embodiment 4,7 three sample XRD spectrums of embodiment compare；
Product made from embodiment 1 is single-phase, and all diffraction maximums belong to Mg in its XRD spectrum21-28In28-34P42-48Oy。
As shown in Figure 1, embodiment 4, the diffraction maximum and the position consistency of the diffraction maximum of embodiment 1 of product obtained by embodiment 7, and do not have
Miscellaneous peak occurs, it is known that the product obtained by embodiment 4, embodiment 7 is single-phase.
Fig. 4 is Mg made from embodiment 4~621-28(In1-xEux)28-34P42-48OyThe exciting light spectrogram of fluorescent material；
It is 598nm by fixed transmission wavelength, the excitation spectrum of fluorescent material made from measurement embodiment 4~6 can from figure
To find out, it is located in the range of 200~500nm at 200-280nm, 316nm, 360nm, 380nm, 392nm and 463nm and occurs
Excitation peak, wherein the width in the range of 200-280nm excites peak intensity to be significantly stronger than other excitation peaks；It is obvious that implementing
The intensity of fluorescent material PLE made from example 4 is higher than fluorescent material made from embodiment 5 and 6.
Fig. 5 is Mg made from embodiment 4~621-28(In1-xEux)28-34P42-48OyThe launching light spectrogram of fluorescent material；
According to the excitation peak feature of embodiment in Fig. 4 4~6, fixed excitation wavelength is 234nm, and measurement embodiment 4~6 is made
Fluorescent material emission spectrum, it can be seen that in the range of 525~720nm be located at 590nm, 599nm, 609nm,
Occurs emission peak at 614nm, 623nm, 651nm, 660nm, 687nm and 707nm, the transmitting peak intensity at 595nm is obvious
It is better than other positions diffraction maximum；It is made it is obvious that the intensity that phosphor emission made from embodiment 4 is composed is higher than embodiment 5 and 6
Fluorescent material.
Wherein, requirement of the three-color fluorescent lamp to fluorescent material be：Maximum excitation wavelength is in 254nm or so.According to Fig. 4 and figure
5 understand that fluorescent material made from embodiment 4~6 can apply to the red color components of three-color fluorescent lamp.
Mg made from Fig. 6 embodiments 7~921-28(In1-xTbx)28-34P42-48OyThe exciting light spectrogram of fluorescent material；
It is 541nm by fixed Tb characteristic emission wavelengths, the excitation spectrum of fluorescent material made from measurement embodiment 7~9, from
It can be seen from the figure that, is located at 200~237nm, 237~285nm and 330~386nm in the range of 200~500nm and occurs
Excitation peak, wherein the width in the range of 200~285nm excites peak intensity to be significantly stronger than other excitation peaks；It is obvious that implementing
The intensity of fluorescent material PLE made from example 7 is higher than fluorescent material made from embodiment 8 and 9.
Fig. 7 is Mg made from embodiment 7~921-28(In1-xEux)28-34P42-48OyThe launching light spectrogram of fluorescent material；
It is 228nm, fluorescence made from measurement embodiment 7~9 to fix excitation wavelength according to the excitation peak of embodiment in Fig. 6 7~9
The emission spectrum of powder, it can be seen that in the range of 350~680nm be located at 378nm, 411nm, 437nm, 490nm,
Occurs emission peak at 500nm, 541nm, 548nm, 585nm, 599nm and 624nm, the emission peak at 541nm is highest peak；
It is obvious that the intensity that phosphor emission made from embodiment 7 is composed is higher than fluorescent material made from embodiment 8 and 9.
Wherein, requirement of the three-color fluorescent lamp to fluorescent material be：Maximum excitation wavelength is in 254nm or so.According to Fig. 6 and figure
7 understand that fluorescent material made from embodiment 7~9 can apply to the green components of three-color fluorescent lamp.
Fig. 8 is embodiment 4, the chromaticity coordinate figure of fluorescent material made from embodiment 7；
Chromaticity coordinate analysis is carried out to the fluorescent material using cie color software, embodiment 4, the chromaticity coordinate of embodiment 7 is determined
Respectively (0.6167,0.3827), (0.3050,0.5506).
Fig. 9 is the fluorescence lifetime curve of fluorescent material made from embodiment 4；
Experiment value is represented by carrying out circle in fluorescence lifetime test, figure to the fluorescent material, solid line is fitting data, fitting
Data fit formula y=A1*exp(-x/t1)+y0, the fluorescence lifetime for calculating fluorescent material is 6.252ms.
Figure 10 is the fluorescence lifetime curve of fluorescent material made from embodiment 7；
Experiment value is represented by carrying out circle in fluorescence lifetime test, figure to the fluorescent material, solid line is fitting data, fitting
Data fit formula y=A1*exp(-x/t1)+A2*exp(-x/t2)+y0, pass through weighted formula τ=(A1*t1 2+A2*t2 2)/(A1*
t1+A2*t2), the fluorescence lifetime for calculating fluorescent material is 7.302ms.
Embodiment：
The present invention is intended to further illustrate with reference to embodiments, is not intended to limit the present invention.
Embodiment 1：Mg25In30P45O182.5The preparation of fluorescent material matrix
Weigh 0.1947g MgO, 0.8049g In2O3、1.0004g NH4H2PO4It is placed in beaker, adding appropriate nitric acid makes
Dissolution of raw material, adds a small amount of polyvinyl alcohol and appropriate amount of deionized water, heating stirring puts beaker to being evaporated completely after solution clarification
Ground after being dried in drying box uniform；Two steps are carried out afterwards burns (1200 DEG C of first stage sintering temperature, after being incubated 15 hours eventually
With room temperature is furnace-cooled to, grind 10 minutes；1200 DEG C of second stage sintering temperature, insulation cools to room temperature, two with the furnace after 15 hours
Step sintering heating rate is 5 DEG C/min).Burned sample is taken out and ground, you can Mg is made25In30P45O182.5Fluorescent material
Matrix.Through indexing, its cell parameter is：α=104.4420 °,
109.8360 °, γ=100.3720 °,Z=1.
Embodiment 2：Mg23In29P44O176.5The preparation of fluorescent material matrix
Weigh 0.1851g MgO, 0.8040g In2O3、1.0108g NH4H2PO4, remaining step is same as Example 1.
Embodiment 3：Mg27In33P47O194The preparation of fluorescent material matrix
Weigh 0.1965g MgO, 0.8272g In2O3、0.9763g NH4H2PO4, remaining step is same as Example 1.
Embodiment 4：Mg25(In0.98Eu0.02)30P45O182.5The preparation of fluorescent material
Weigh 0.1943g MgO, 0.7871g In2O3、0.0204g Eu2O3、0.9982g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 5：Mg25(In0.95Eu0.05)30P45O182.5The preparation of fluorescent material
Weigh 0.1937g MgO, 0.7605g In2O3、0.0507g Eu2O3、0.9950g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 6：Mg25(In0.91Eu0.09)30P45O182.5The preparation of fluorescent material
Weigh 0.1929g MgO, 0.7254g In2O3、0.0909g Eu2O3、0.9908g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 7：Mg25(In0.93Tb0.07)30P45O182.5The preparation of fluorescent material
Weigh 0.1929g MgO, 0.7413g In2O3、0.0751g Tb4O7、0.9907g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 8：Mg25(In0.95Tb0.05)30P45O182.5The preparation of fluorescent material
Weigh 0.1934g MgO, 0.7593g In2O3、0.0538g Tb4O7、0.9935g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 9：Mg25(In0.91Tb0.09)30P45O182.5The preparation of fluorescent material
Weigh 0.1923g MgO, 0.7234g In2O3、0.0963g Tb4O7、0.9880g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Comparative example 1：Mg：In：P mol ratios are 33.3：22.2：The preparation of 44.5 sample
Weigh 0.2816g MgO, 0.6467g In2O3、1.0717g NH4H2PO4, remaining step is same as Example 1.
Comparative example 2：Mg：In：P mol ratios are 23：37：The preparation of 40 sample
Weigh 0.1739g MgO, 0.9633g In2O3、0.8629g NH4H2PO4, remaining step is same as Example 1.
Comparative example 3：Mg：In：P mol ratios are 30：28：The preparation of 42 sample
Weigh 0.2436g MgO, 0.7831g In2O3、0.9733g NH4H2PO4, remaining step is same as Example 1.
Claims (8)
1. a kind of fluorescent RE powder magnesium Indium phosphate host material, it is characterised in that be using chemical formula as Mg21-28In28- 34P42-48OyFor the matrix of RE phosphate fluorescent material, wherein y is molal quantity, y=168-199.
2. a kind of fluorescent RE powder according to claim 1 magnesium Indium phosphate host material, it is characterised in that the phosphorus
Hydrochlorate Mg21-28In28-34P42-48OyMatrix belongs to anorthic system, and space group is
3. the preparation method of the fluorescent RE powder magnesium Indium phosphate host material described in claim 1 or 2, by Mg:In:P rubs
You are than being 21-28:28-34:42-48, weighs raw material MgO, In2O3And NH4H2PO4, made with wet-chemical-solid-phase synthesis synthesis
It is standby.
4. the preparation method of the fluorescent RE powder magnesium Indium phosphate host material described in claim 3, it is characterized in that：According to change
Formula is Mg21-28In28-34P42-48OyRequired nonstoichiometric molar ratio weighs raw material MgO, In2O3And NH4H2PO4, adding strong acid makes
Dissolution of raw material, adds polyvinyl alcohol and deionized water, heating stirring grinds dried material to being evaporated completely after solution clarification
Mill is uniform；First stage sintering is carried out at 1100-1300 DEG C, grinding at room temperature is cooled to, then in 1100-1300 DEG C of temperature strip
Second stage sintering is carried out under part, grinding obtains final product after cooling.
5. preparation method according to claim 4, it is characterised in that the heating rate of first stage sintering for 3~7 DEG C/
min。
6. preparation method according to claim 4, it is characterised in that the heating rate of second stage sintering for 3~7 DEG C/
min。
7. preparation method according to claim 4, it is characterised in that 10~20h of soaking time of first stage sintering.
8. preparation method according to claim 4, it is characterised in that 10~20h of soaking time of second stage sintering.
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| CN113185974B (en) * | 2020-01-14 | 2022-11-08 | 中南大学 | Indium strontium pyrophosphate fluorescent matrix material, fluorescent material, and preparation and application thereof |
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