CN105800584B - A kind of fluorescent RE powder phosphate base material and preparation method thereof - Google Patents
A kind of fluorescent RE powder phosphate base material and preparation method thereof Download PDFInfo
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- CN105800584B CN105800584B CN201610153433.XA CN201610153433A CN105800584B CN 105800584 B CN105800584 B CN 105800584B CN 201610153433 A CN201610153433 A CN 201610153433A CN 105800584 B CN105800584 B CN 105800584B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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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
- C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
- C09K11/71—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus also containing alkaline earth metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Abstract
The invention provides a kind of fluorescent RE powder phosphate base material and preparation method thereof, its chemical composition is Mg14~ 19In23~32P54~62Oy(y=183~222).The preparation method uses wet-chemical solid sintering technology.The present invention be successfully prepared first obtain it is a kind of it is new can as phosphor host phosphate compounds, wherein containing the phosphide element with rare earth element property, rare earth element enters in parent lattice as Validation Counter, thus the compound that the present invention is prepared can be as fluorescent material host material.
Description
Technical field：
The present invention relates to rare earth luminescent material field, more particularly, to a kind of fluorescent RE powder with phosphate base material and
Its preparation method.
Background technology：
Fluorescent material is the powder polycrystalline material that can be lighted under certain shooting condition.In information age today, fluorescent material is
As material indispensable in people's daily life, it is widely used in computer monitor, television screen, mobile phone and shown
The numerous areas such as screen, indoor and outdoor lighting, decoration, hospital's Chest X-rays equipment, airport security, Fire Alarm, currency security mark.Base
Matter is the important component of fluorescent material, and different matrix are because of its crystal structure difference, the crystal being subject to after active ions doping
Field action also difference, and then influence engery level cracking, macroscopically shows as the difference of spectral quality.Phosphate is because of its phonon energy
Amount is moderate, has in VUV-ultraviolet region compared with strong absorption band, and the solubility to rare earth ion is high, and with physical chemistry
The advantages of performance stabilization, low raw-material cost, simple preparation technology, be a kind of important phosphor host, with very high
Application value.Using phosphate as matrix, incorporation rare earth ion can be prepared by RE phosphate fluorescent material as exciting agent, be property
One of fluorescent material that can be excellent.Since the seventies of last century six, both at home and abroad to the spy using phosphate as the fluorescent material of matrix
Rope is also constantly being carried out, and is 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.From the point of view of anion structure, wherein research more application compared with
It is wide mainly around orthophosphates (PO4)nWith pyrophosphate (P2O7)nSeries, its matrix does not light in itself, but VUV-
There is stronger absorption near ultraviolet band, and this charge migration just between rare earth ion-coordination oxygen matches, can be effectively by energy
Amount passes to the centre of luminescence, and radiates in the form of light.Research work is surrounded based on mostly in the current field
Have been reported that the doping vario-property of compound and deploy, or a series of isostructural compoundses compared with mature substrate are studied, and visit
The work of rope New-type matrix material is then relatively rare.A kind of noval chemical compound is from synthesis pure sample is found to, and its composition proportion etc. is all needed
Explore and determine by many experiments；In addition, simultaneously not all compound is suitable as fluorescent material host material, it is desirable to which it has
There are the characteristics such as absorption visible region high transmission, thus people in the art in good heat endurance and chemical stability, ultra-violet (UV) band
Member is it is generally acknowledged that the process for exploring new host material is very difficult.
The content of the invention：
The purpose of the present invention aims to provide a kind of new fluorescent RE powder phosphate base material.
Another object of the present invention is to there is provided the simple its preparation process of above-mentioned material.
The phosphate matrix composition expression formula Mg of the present invention14~19In23~32P54~62Oy(y=183~222), are rare earth phosphorus
The matrix of hydrochlorate fluorescent material, wherein y are molal quantity, y=183~222.
Described phosphate matrix crystal belongs to monoclinic system, C2/c (No.15) space group.
The phosphate matrix materials process that the present invention is synthesized is, according to Mg:In:P mol ratios are (14~19):(23~
32):(54~62), can weigh raw material MgO, In2O3And NH4H2PO4, and prepared according to wet-chemical-solid-phase synthesis of the present invention
Technique, can obtain Mg14~19In23~32P54~62Oy(y=183~222) fluorescent material phosphate base material.
The present invention prepares fluorescent material using wet-chemical-solid phase reaction method, by Mg:In:P mol ratio for (14~
19):(23~32):(54~62) weigh appropriate MgO, In2O3And NH4H2PO4It is put into beaker, adds strong acid (such as nitric acid
Deng), heating stirring makes dissolution of raw material, (can also be that other chemistry are pure after addition polyvinyl alcohol and deionized water after solution clarification
The high water quality of degree), dried material is ground uniform by heating stirring to being evaporated completely；First is carried out at 900-1200 DEG C
Stage is sintered, and is cooled to room temperature, grinds, and second stage sintering is then carried out under 900-1200 DEG C of temperature conditionss, and cooling is ground
Mill, obtains final product.
The heating rate of first stage sintering step is preferably 3~7 DEG C/min；
The heating rate of second stage sintering step is preferably 3~7 DEG C/min；
The soaking time of first stage sintering step is preferably 10~20 hours；
The soaking time of second stage sintering step is preferably 10~20 hours.
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 studying15In30P60O210(=MgIn2P4O14), because Mg/In/P exists
Mutually there is certain solid solubility, its actual solid solution molecular formula is Mg in lattice14~19In23~32P54~62Oy.Utilize the present invention's
The X-ray powder diffraction data of host material, using Fullprof softwares carry out indexing, show that the material belongs to monoclinic crystal
System, C2/c (No.15) space group.Inventor by host material of the present invention by comparing joint committee (ICDD)
Powder diffraction data storehouse (PDF-4+2011) and Inorganic crystal structure database (ICSD) and the softwares of MDI jade 5.0, can be true
Fixed matrix of the present invention is a kind of crystal structure compound that there is not been reported.
Beneficial effects of the present invention
The present invention be successfully prepared first obtain it is a kind of it is new can as phosphor host phosphate chemical combination
Thing, wherein containing the phosphide element with rare earth element property, rare earth element enters in parent lattice as Validation Counter, 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 1-4 XRD spectrum compares；
In Fig. 1 it is unmarked go out diffraction maximum correspondence the present invention Mg14~19In23~32P54~62OyDiffraction maximum.Can be with from figure
Find out, embodiment 1, contain Mg in the sample XRD spectrum obtained by comparative example 1-414~19In23~32P54~62OyDiffraction maximum is right
Product made from 1~comparative example of ratio 4 is mixed phase, and the product obtained by embodiment 1 is Mg in the present invention14~19In23~ 32P54~62OyThe single phase composition sample of phosphor host.
Fig. 2 is MgO-InO where embodiment 1,2,3, comparative example 1-41.5-PO2.5The rich phosphorus end phasor of ternary system；Wherein
The composition of embodiment 1,2,3 is designated as 1,6,7, and comparative example 1-4 composition is designated as 2,3,4,5；
The phasor is to be based on material phase analysis result in embodiment 1,2,3, comparative example 1-4, according to phase rule in composition triangle
Middle drafting is obtained.Mg in the present invention is represented in figure at ellipse14~19In23~32P54~62OyWhere (y=183~222) host material
Composition it is interval, the composition of 1~comparative example of comparative example 4 is outside the interval, and embodiment 2, embodiment 3 are leaned on into branch in the interval
At proximal border.
Fig. 3 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 invention14~19In23~32P54~62OyThe single phase composition of phosphor host
Sample.
Fig. 4 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 spectrum14~19In23~32P54~ 62Oy.As shown in Figure 4, embodiment 4, the diffraction maximum and the position consistency of the diffraction maximum of embodiment 1 of product obtained by embodiment 7, and
There is no miscellaneous peak appearance, it is known that the product obtained by embodiment 4, embodiment 7 is single-phase.
Fig. 5 is Mg made from embodiment 4~614~19(In1-xEux)23~32P54~62OyThe exciting light spectrogram of fluorescent material；
It is 618nm 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, 361nm, 380nm, 392nm, 413nm and 464nm 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. 6 is Mg made from embodiment 4~614~19(In1-xEux)23~32P54~62OyThe launching light spectrogram of fluorescent material；
According to the excitation peak feature of embodiment in Fig. 6 4~6, fixed excitation wavelength is 240nm, 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 595nm, 618nm, 656nm,
Occur emission peak at 686nm, 700nm and 707nm, increase with doping concentration, the transmitting peak intensity at 595nm exceedes
Turn into highest peak at 618nm；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. 5 and figure
6 understand that fluorescent material made from embodiment 4~6 can apply to the red color components of three-color fluorescent lamp.
Fig. 7 is Mg made from embodiment 7~914~19(In1-xTbx)23~32P54~62OyThe exciting light spectrogram of fluorescent material；
It is 548nm 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, 237~261nm, 265nm, 301nm, 316nm in the range of 200~500nm
With excitation peak is occurred in that at 330~386nm, wherein to excite peak intensity to be significantly stronger than other for the width in the range of 200~261nm
Excitation peak；It is obvious that the intensity of fluorescent material PLE made from embodiment 7 is higher than fluorescent material made from embodiment 8 and 9.
Fig. 8 is Mg made from embodiment 7~914~19(In1-xTbx)23~32P54~62OyThe launching light spectrogram of fluorescent material；
It is 246nm, fluorescence made from measurement embodiment 7~9 to fix excitation wavelength according to the excitation peak of embodiment in Fig. 8 7~9
The emission spectrum of powder, it can be seen that in the range of 350~700nm be located at 319nm, 416nm, 437nm, 541nm,
Occur emission peak at 548nm, 584nm, 599nm and 622nm, increase with doping concentration, the emission peak at 548nm is most strong
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.
Fig. 9 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 (0.6300,0.3691), (0.3268,0.5239).
Figure 10 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 3.533ms.
Figure 11 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)+y0, the fluorescence lifetime for calculating fluorescent material is 4.676ms.
Embodiment：
The present invention is intended to further illustrate with reference to embodiments, is not intended to limit the present invention.
Embodiment 1：Mg17In27P56O197.5The preparation of fluorescent material matrix
Weigh 0.1260g MgO, 0.6893g In2O3、1.1847g 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 (1000 DEG C of first stage sintering temperature, after being incubated 15 hours eventually
With room temperature is furnace-cooled to, grind 10 minutes；1000 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 made17In27P56O197.5Fluorescent material
Matrix.Through indexing, its cell parameter is：β=108.39
(0)°,Z=4.
Comparative example 1：Mg：In：P mol ratios are 10：32：The preparation of 58 sample
Weigh 0.0700g MgO, 0.7714g In2O3、1.1586g NH4H2PO4, remaining step is same as Example 1.
Comparative example 2：Mg：In：P mol ratios are 13：26：The preparation of 60 sample
Weigh 0.0950g MgO, 0.6542g In2O3、1.2509g NH4H2PO4, remaining step is same as Example 1.
Comparative example 3：Mg：In：P mol ratios are 20：20：The preparation of 60 sample
Weigh 0.1538g MgO, 0.5296g In2O3、1.3166g NH4H2PO4, remaining step is same as Example 1.
Comparative example 4：Mg：In：P mol ratios are 23：24：The preparation of 53 sample
Weigh 0.1819g MgO, 0.6373g In2O3、1.1808g NH4H2PO4, remaining step is same as Example 1.
Embodiment 2：Mg14In23P54O183.5The preparation of fluorescent material matrix
Weigh 0.1132g MgO, 0.6406g In2O3、1.2462g NH4H2PO4, remaining step is same as Example 1.
Embodiment 3：Mg18.5In29.5P58O207.75The preparation of fluorescent material matrix
Weigh 0.1295g MgO, 0.7114g In2O3、1.1590g NH4H2PO4, remaining step is same as Example 1.
Embodiment 4：Mg17(In0.93Eu0.07)27P56O197.5The preparation of fluorescent material
Weigh 0.1277g MgO, 0.6370g In2O3、0.0608g Eu2O3、1.2006g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 5：Mg17(In0.95Eu0.05)27P56O197.5The preparation of fluorescent material
Weigh 0.1279g MgO, 0.6518g In2O3、0.0435g Eu2O3、1.2028g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 6：Mg17(In0.89Eu0.11)27P56O197.5The preparation of fluorescent material
Weigh 0.1272g MgO, 0.6073g In2O3、0.0951g Eu2O3、1.1962g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 7：Mg17(In0.93Tb0.07)27P56O197.5The preparation of fluorescent material
Weigh 0.1275g MgO, 0.6358g In2O3、0.0644g Tb4O7、1.1983g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 8：Mg17(In0.95Tb0.05)27P56O197.5The preparation of fluorescent material
Weigh 0.1278g MgO, 0.6510g In2O3、0.0461g Tb4O7、1.2012g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 9：Mg17(In0.91Tb0.09)27P56O197.5The preparation of fluorescent material
Weigh 0.1272g MgO, 0.6206g In2O3、0.0826g Tb4O7、1.1955g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Claims (7)
1. a kind of fluorescent RE powder phosphate base material, it is characterised in that be using chemical formula as Mg14~19In23~32P54~62Oy
For the matrix of RE phosphate fluorescent material, wherein y is molal quantity, y=183 ~ 222.
2. a kind of fluorescent RE powder phosphate material according to claim 1, it is characterised in that the phosphate
Mg14~19In23~32P54~62OyMatrix belongs to monoclinic system, and space group isC2/c (No.15)。
3. the preparation method of the fluorescent RE powder phosphate base material described in claim 1 or 2, by Mg:In:P mol ratios
For 14 ~ 19:23~32:54 ~ 62, weigh raw material MgO, In2O3And NH4H2PO4, system synthetically prepared with wet-chemical-solid-phase synthesis
It is for process：It is Mg according to chemical formula14~19In23~32P54~62OyRequired nonstoichiometric molar ratio weighs raw material MgO, In2O3With
NH4H2PO4, adding strong acid makes dissolution of raw material, and polyvinyl alcohol and deionized water, heating stirring to complete steaming are added after solution clarification
It is dry, dried material is ground uniform；First stage sintering is carried out at 900-1200 DEG C, room temperature is cooled to, ground, then
Second stage sintering is carried out under 900-1200 DEG C of temperature conditionss, grinding obtains final product after cooling.
4. preparation method according to claim 3, it is characterised in that the heating rate of first stage sintering for 3 ~ 7 DEG C/
min。
5. preparation method according to claim 3, it is characterised in that the heating rate of second stage sintering for 3 ~ 7 DEG C/
min。
6. preparation method according to claim 3, it is characterised in that 10 ~ 20h of soaking time of first stage sintering.
7. preparation method according to claim 3, it is characterised in that 10 ~ 20h of soaking time of second stage sintering.
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| CN112708420B (en) * | 2019-10-24 | 2023-04-25 | 中南大学 | Indium strontium pyrophosphate fluorescent matrix material, fluorescent material, preparation and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101824322A (en) * | 2009-03-05 | 2010-09-08 | 建兴电子科技股份有限公司 | Fluorescent material and fluorescent lamp applying the same |
| CN105176529A (en) * | 2015-09-19 | 2015-12-23 | 青岛科技大学 | Europium-manganese coactivated phosphate white light fluorescent powder and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101824322A (en) * | 2009-03-05 | 2010-09-08 | 建兴电子科技股份有限公司 | Fluorescent material and fluorescent lamp applying the same |
| CN105176529A (en) * | 2015-09-19 | 2015-12-23 | 青岛科技大学 | Europium-manganese coactivated phosphate white light fluorescent powder and preparation method thereof |
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