CN105860973A - Magnesium-indium phosphate red and green fluorescent powder and preparation method thereof - Google Patents

Magnesium-indium phosphate red and green fluorescent powder and preparation method thereof Download PDF

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CN105860973A
CN105860973A CN201610235078.0A CN201610235078A CN105860973A CN 105860973 A CN105860973 A CN 105860973A CN 201610235078 A CN201610235078 A CN 201610235078A CN 105860973 A CN105860973 A CN 105860973A
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powder
fluorescent powder
preparation
fluorescent material
phosphate
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CN105860973B (en
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蔡格梅
张静
司家勇
金展鹏
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Central South University
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/70Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
    • C09K11/71Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus also containing alkaline earth metals
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7728Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
    • C09K11/7737Phosphates
    • C09K11/7738Phosphates with alkaline earth metals
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7743Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing terbium
    • C09K11/7752Phosphates
    • C09K11/7753Phosphates with alkaline earth metals

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  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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Abstract

The invention provides magnesium-indium phosphate red and green fluorescent powder and a preparation method thereof. The chemical formula of the magnesium-indium phosphate red and green fluorescent powder is Mg21-28(In1-xLnx)28-34P42-48Oy (x=0.02-0.11, y=168-199), wherein Ln is rare earth ion Eu or Tb. In the fluorescent powder, a novel phosphate compound Mg21-28In28-34P42-48Oy (y=168-199) is used as a substrate, different rare earth elements are added into the substrate, and therefore the fluorescent material having strong emission in different spectral regions under ultraviolet excitation can be obtained. The preparation method is a wet-chemical-solid phase sintering method. The fluorescent powder has good optical performance and can well meet the requirements of a three-band-color fluorescent lamp.

Description

A kind of magnesium Indium phosphate is red or green emitting phosphor and preparation thereof
Technical field:
The present invention relates to rare earth luminescent material field, the one especially relating to can apply to three-color fluorescent lamp is red or green RE phosphate base fluorescent powder and preparation method thereof.
Background technology:
Current commercial light source major part needs to use fluorescent material to make light conversion, rare-earth trichromatic fluorescent powder the fluorescent lamp right and wrong prepared The most energy-efficient new type light source, is the prior development direction of world's lighting source.All kinds of rare earth luminescent material of China produces at present Ability has reached ten thousand tons, 2009, and China produces all kinds of fluorescent RE powder about 7200 tons altogether, and rare-earth trichromatic fluorescent lamp yield surpasses Cross 3,000,000,000, rank first in the world.Three-color fluorescent lamp (electricity-saving lamp) accounts for the 75% of rare earth luminescent material, is the most luminous material One of main application fields of material, and owing to three-color fluorescent lamp has the advantages such as energy-conservation, long-life than incandescent lamp, future will be by Step eliminates incandescent lamp, becomes the fresh combatants of lamp ornaments lighting industry.Rare-earth trichromatic fluorescent powder then possess ultraviolet radiation stability can good, The sudden temperature advantages of higher of heat, its finished product rare-earth trichromatic fluorescent lamp has specular removal, low light attenuation, long-life feature.Phosphate Because its phonon energy is moderate, there is stronger absorption band in VUV-ultraviolet (VUV-UV) region, be suitable for rear-earth-doped luminescence, And have that luminous efficiency is high, physical and chemical performance is stable, raw material is easy to get and cheap, advantage, the tool such as preparation technology is simple There is the highest using value.With phosphate as matrix, mix rare earth ion and can be prepared by RE phosphate fluorescent material as exciting agent. From the research of conventional all kinds of system fluorescent material it is seen that, Eu3+It is to apply more ruddiness active ions, Tb3+It is then to apply relatively Many green glow active ions.Since last century six the seventies, both at home and abroad to the exploration of the fluorescent material with phosphate as matrix also Constantly carrying out, be prepared for a series of RE phosphate fluorescent material (LaPO that can be used 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 is wider Mainly around orthophosphates (PO4)nWith pyrophosphate (P2O7)nSeries, its matrix itself is the most luminous, but purple at VUV-closely Outskirt has stronger absorption, and this just matches with the charge migration between rare earth ion-coordination oxygen, can effectively be transmitted by energy To the centre of luminescence, and radiate in the form of light.In this field, research work is all around based on having been reported mostly at present The doping vario-property of compound and launch, or a series of isostructural compoundses compared with mature substrate are studied, and explore new medium The work of material is the most rare.A kind of noval chemical compound is from being found to synthesis pure sample, and its composition proportion etc. all needs through great many of experiments Exploration determines;It addition, and not all compound be suitable as fluorescent material host material, it is desirable to it has good thermally-stabilised (fluorescent material does not decomposes or is not easy and device for property (fluorescent material does not changes in room temperature long-time performance used above) and chemical stability Part reacts), the characteristic such as visible light-transmissive strong to UV Absorption be high, thus those skilled in the art it is generally acknowledged that exploration makes new advances matrix The process of material is the most difficult.
Summary of the invention:
The purpose of the present invention aims to provide the redness of a kind of new host material or green single-phase RE phosphate phosphor material, has Good optical property, and the requirement of three-color fluorescent lamp can be met very well.
Another object of the present invention is to, it is provided that the simple its preparation process of above-mentioned material.
The single-phase redness of the present invention or the chemical formula of green rare-earth phosphate phosphor material are Mg21-28(In1-xLnx)28-34P42-48Oy, Ln=Eu or Tb, x, y are molal quantity, wherein x=0.02~0.11, y=168~199.
Inventor finds Mg by research21-28(In1-xEux)28-34P42-48OyEffective excitation wavelength be positioned at 210~280nm scopes In, for red fluorescence powder.Mg21-28(In1-xTbx)28-34P42-48OyEffective excitation wavelength be positioned at 210~280nm in the range of, For green emitting phosphor.
The present invention is first by new for one phosphate matrix, for fluorescent material, and this matrix components expression formula Mg21-28In28-34P42-48Oy (y=168~199).This crystal belongs to anorthic system, P-1 (No.2) space group.Mix a small amount of active ions Ln3+(Ln=Eu or Tb) Substitute For Partial In3+, can be prepared by redness or green Mg21-28(In1-xLnx)28-34P42-48Oy(x=0.02~0.11, y=168~199) Fluorescent material.
The phosphate compounds of the present invention wherein contains phosphide element, and therefore rare earth element is easy to be replaced by part as Validation Counter Mode for phosphide element enters in parent lattice, thus the compound that the present invention prepares can be as fluorescent material host material; In prior art, there is not been reported for this magnesium Indium phosphate host material prepared of the present invention.Utilize the host material of the present invention X-ray powder diffraction data, employing Fullprof software carry out indexing, show that this material belongs to anorthic system, P-1 (No.2) Space group.Inventor is by by host material comparison joint committee (ICDD) powder diffraction data storehouse of the present invention (PDF-4+2011) and Inorganic crystal structure database (ICSD) and MDI jade 5.0 software, it may be determined that matrix of the present invention For the compound that a kind of crystal structure that there is not been reported is brand-new.
Using wet-chemical-solid-phase sintering method to carry out polycrystal synthesis in the present invention, detailed process is as follows: because this fluorescent material matrix Material is a kind of novel solid solution compound unknown without report and structure, and its ideal linearity molecular formula is Mg3In4P6O24, by Mutually there is in lattice certain solid solubility scope therefore in Mg/In/P, its actual solid solution molecular formula Mg21-28In28-34P42-48Oy
When using wet-chemical-solid phase reaction method to prepare fluorescent material sample, by Mg:(In1-xLnx): the mol ratio of P is (21~28): (28~34): (42~48) weigh appropriate MgO, In2O3(Eu2O3/Tb4O7) and NH4H2PO4Put in beaker, add Strong acid (such as nitric acid etc.), adds thermal agitation and makes dissolution of raw material, adds polyvinyl alcohol and deionized water, add thermal agitation after solution is clarified To being evaporated completely, grind after drying uniformly;At 1100-1300 DEG C, carry out first stage sintering, be cooled to room temperature, grind, Then under 1100-1300 DEG C of temperature conditions, carry out second stage sintering, cooling, grind, obtain end product.
In preparation process of the present invention, 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 temperature retention time of first stage sintering step is preferably 10~20 hours;
In preparation process of the present invention, the temperature retention time of second stage sintering step is preferably 10~20 hours.
The XRD result of the present invention shows the crystal structure of the rare earth doping fluorescent powder sample that the method synthesizes and the pure of undoped Compare and do not change.
In concrete research process, explore according to great many of experiments and determine, according to Mg:(In1-xLnx): P mol ratio is (21~28): (28~34): (42~48) weigh raw material MgO, In2O3(Eu2O3/Tb4O7) and NH4H2PO4, and according to the humidifying of the present invention -solid-phase synthesis preparation technology, it is possible to obtain the x=0.02 of the present invention~the Mg of 0.1121-28(In1-xLnx)28-34P42-48OyProduct.
Beneficial effects of the present invention
The present invention successfully explores a kind of new phosphate compounds as the redness of phosphor host and green emitting phosphor, and In prior art, there is not been reported for phosphor material powder with magnesium Indium phosphate as matrix;Fluorescent material obtained by the present invention has at purple Outskirt Absorber Bandwidth (200~280nm wave-length coverage), it is seen that light district transmitance is high, luminous intensity height, good stability, preparation The features such as technique is simpler.
Two kinds of Novel phosphoric acid salt base fluorescent powders that the present invention prepares.Wherein Mg21-28(In1-xEux)28-34P42-48OyMost preferably excite Wavelength is positioned at about 234nm, launches the most by force wavelength and is positioned at 589nm and 599nm, meets electricity-saving lamp red fluorescence powder Condition;Such fluorescent material is carried out attenuation curve test analysis and finds that its fluorescence lifetime is at about 6.2ms. Mg21-28(In1-xTbx)28-34P42-48OyMaximum excitation wavelength is positioned at about 228nm and 251nm, launches the most by force wavelength and is positioned at Near 541nm, well meet the condition of energy-conservation green-fluorescent powder for lamp;Such fluorescent material is carried out attenuation curve test point Analysis finds that its fluorescence lifetime is at about 7.3ms.The fluorescent material of the present invention is suitable in three-color fluorescent lamp.
Light-emitting phosphor intensity prepared by the present invention is high, the sunset glow time is short, effectively can be excited by 200~270nm light.It addition, this The preparation method of invention needs the equipment of employing and synthesis technique simple, is suitable for large-scale industrial production, and these features are just full The requirement of foot three-color fluorescent lamp.
Accompanying drawing illustrates:
Fig. 1 is embodiment 1, and the XRD spectrum of comparative example 1-3 compares;
In Fig. 1 unmarked go out the Mg of the diffraction maximum correspondence present invention21-28In28-34P42-48OyDiffraction maximum.It can be seen that Embodiment 1, all contains Mg in the sample XRD spectrum obtained by comparative example 1-321-28In28-34P42-48OyDiffraction maximum, comparative example 1~the product for preparing of comparative example 3 be 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 be embodiment 1, embodiment 2,3 three samples of embodiment XRD spectrum compare;
It can be seen that the sample XRD spectrum that embodiment 2, embodiment 3 prepare is composed with embodiment 1 sample XRD Completely the same, do not have miscellaneous peak to occur, be all Mg in the present invention21-28In28-34P42-48OyThe single-phase composition of phosphor host Sample.
Fig. 3 is embodiment 1, embodiment 4, and 7 three sample XRD spectrums of embodiment compare;
The product that embodiment 1 prepares is single-phase, and in its XRD spectrum, all diffraction maximums belong to Mg21-28In28-34P42-48Oy.By Fig. 1 understands, the diffraction maximum of the product obtained by embodiment 4, embodiment 7 and the position consistency of embodiment 1 diffraction maximum, and does not has Miscellaneous peak is had to occur, it is known that the product obtained by embodiment 4, embodiment 7 is single-phase.
Fig. 4 is the Mg that embodiment 4~6 prepares21-28(In1-xEux)28-34P42-48OyThe exciting light spectrogram of fluorescent material;
It is 598nm by fixed transmission wavelength, measures the excitation spectrum of the fluorescent material that embodiment 4~6 prepares, can from figure Go out, in the range of 200~500nm, be positioned at 200-280nm, 316nm, 360nm, 380nm, 392nm and 463nm Place occurs in that excitation peak, is wherein positioned at the wide excitation peak intensity in the range of 200-280nm and is significantly stronger than other excitation peak;It is obvious that The intensity of the fluorescent material PLE that embodiment 4 prepares is higher than the fluorescent material that embodiment 5 and 6 prepares.
Fig. 5 is the Mg that embodiment 4~6 prepares21-28(In1-xEux)28-34P42-48OyThe emission spectrum figure of fluorescent material;
According to embodiment in Fig. 4 4~6 excitation peak feature, fixing excitation wavelength is 234nm, and it is glimmering that measurement embodiment 4~6 prepares The emission spectrum of light powder, it can be seen that be positioned in the range of 525~720nm 590nm, 599nm, 609nm, Emission peak occurs at 614nm, 623nm, 651nm, 660nm, 687nm and 707nm, is positioned at the transmitting at 595nm Peak intensity is significantly stronger than other position diffraction maximums;It is obvious that the intensity that the phosphor emission that embodiment 4 prepares is composed is higher than enforcement The fluorescent material that example 5 and 6 prepares.
Wherein, the requirement of fluorescent material is by three-color fluorescent lamp: maximum excitation wavelength is at about 254nm.According to Fig. 4 and Fig. 5 Understanding, the fluorescent material that embodiment 4~6 prepares can apply to the red color components of three-color fluorescent lamp.
The Mg that Fig. 6 embodiment 7~9 prepares21-28(In1-xTbx)28-34P42-48OyThe exciting light spectrogram of fluorescent material;
It is 541nm by fixing Tb characteristic emission wavelength, measures the excitation spectrum of the fluorescent material that embodiment 7~9 prepares, from figure In it can be seen that be positioned in the range of 200~500nm at 200~237nm, 237~285nm and 330~386nm occur Excitation peak, is wherein positioned at the wide excitation peak intensity in the range of 200~285nm and is significantly stronger than other excitation peak;It is obvious that implement The intensity of the fluorescent material PLE that example 7 prepares is higher than the fluorescent material that embodiment 8 and 9 prepares.
Fig. 7 is the Mg that embodiment 7~9 prepares21-28(In1-xEux)28-34P42-48OyThe emission spectrum figure of fluorescent material;
Fixing excitation wavelength according to embodiment in Fig. 6 7~9 excitation peak is 228nm, measures the prepared fluorescent material of embodiment 7~9 Emission spectrum, it can be seen that be positioned in the range of 350~680nm 378nm, 411nm, 437nm, 490nm, Emission peak occurs at 500nm, 541nm, 548nm, 585nm, 599nm and 624nm, is positioned at the transmitting at 541nm Peak is highest peak;It is obvious that the intensity that the phosphor emission that embodiment 7 prepares is composed is higher than the fluorescence that embodiment 8 and 9 prepares Powder.
Wherein, the requirement of fluorescent material is by three-color fluorescent lamp: maximum excitation wavelength is at about 254nm.According to Fig. 6 and Fig. 7 Understanding, the fluorescent material that embodiment 4~6 prepares can apply to the green components of three-color fluorescent lamp.
Fig. 8 is embodiment 4, the chromaticity coordinate figure of the prepared fluorescent material of embodiment 7;
Use cie color software that this fluorescent material is carried out chromaticity coordinate analysis, determine that embodiment 4, embodiment 7 chromaticity coordinate are divided Wei (0.6167,0.3827), (0.3050,0.5506).
Fig. 9 is the fluorescence lifetime curve of the fluorescent material that embodiment 4 prepares;
By this fluorescent material is carried out fluorescence lifetime test, in figure, circle represents experiment value, and solid line is fitting data, fitting data Coincidence formula y=A1*exp(-x/t1)+y0, the fluorescence lifetime calculating fluorescent material is 6.252ms.
Figure 10 is the fluorescence lifetime curve of the fluorescent material that embodiment 7 prepares;
By this fluorescent material is carried out fluorescence lifetime test, in figure, circle represents experiment value, and solid line is fitting data, fitting data Coincidence formula y=A1*exp(-x/t1)+A2*exp(-x/t2)+y0, by weighted formula τ=(A1*t1 2+A2*t2 2)/(A1*t1+A2*t2), The fluorescence lifetime calculating fluorescent material is 7.302ms.
Figure 11 be embodiment 1,4 two samples of comparative example XRD spectrum compare;
Synthetic example 4 sample outside given composition interval, occurs in that Mg in its XRD diffraction spectra3P2O8Second phase, table Bright can not synthesize Mg outside given composition interval21-28In28-34P42-48OySingle-phase sample.
Figure 12 is the emission spectrum figure that embodiment 7,5 two samples of comparative example prepare fluorescent material
Can be evident that from figure, the intensity of the phosphor emission spectrum that embodiment 7 prepares is higher than what comparative example 5 prepared Fluorescent material.
Detailed description of the invention:
It is intended to further illustrate the present invention below in conjunction with embodiment, and the unrestricted 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, adds appropriate nitric acid and make former Material dissolves, and adds a small amount of polyvinyl alcohol and appropriate amount of deionized water, add thermal agitation to being evaporated completely, be placed in by beaker after solution clarification In drying box, dried grinding is uniformly;(first stage sintering temperature 1200 DEG C, after being incubated 15 hours to carry out two steps burning eventually afterwards It is cooled to room temperature with stove, grinds 10 minutes;Second stage sintering temperature 1200 DEG C, cools to room temperature with the furnace after being incubated 15 hours, Two-step sintering heating rate is 5 DEG C/min).Burned sample is taken out and grinds, can be prepared by Mg25In30P45O182.5Fluorescence Powder 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 in 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 in 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 and enforcement Example 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 and enforcement Example 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 and enforcement Example 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 and enforcement Example 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 and enforcement Example 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 and enforcement Example 1 is identical.
Comparative example 1:Mg:In:P mol ratio is the preparation of the sample of 33.3:22.2:44.5
Weigh 0.2816g MgO, 0.6467g In2O3、1.0717g NH4H2PO4, remaining step is same as in Example 1.
Comparative example 2:Mg:In:P mol ratio is the preparation of the sample of 23:37:40
Weigh 0.1739g MgO, 0.9633g In2O3、0.8629g NH4H2PO4, remaining step is same as in Example 1.
Comparative example 3:Mg:In:P mol ratio is the preparation of the sample of 30:28:42
Weigh 0.2436g MgO, 0.7831g In2O3、0.9733g NH4H2PO4, remaining step is same as in Example 1.
It is outer that the comparative example 4:(present invention gives composition range scope) Mg30In28P42O177The preparation of sample
Weigh 0.2413g MgO, 0.7757g In2O3、0.9642g NH4H2PO4, remaining step is same as in Example 1.
It is outer that the comparative example 5:(present invention gives composition range scope) Mg30(In0.93Tb0.07)28P42O177The preparation of sample
Weigh 0.2413g MgO, 0.7214g In2O3、0.0731g Tb4O7、0.9642g NH4H2PO4, remaining step and enforcement Example 1 is identical.

Claims (10)

1. a redness or green rare-earth phosphate phosphor material, it is characterised in that its chemical formula is Mg21-28(In1-xLnx)28-34P42-48OySingle-phase phosphor material powder, wherein Ln=Eu or Tb, x, y are molal quantity, wherein X=0.02~0.11, y=168~199.
A kind of RE phosphate phosphor material powder the most according to claim 1, it is characterised in that this fluorescent material is with phosphoric acid Salt Mg21-28In28-34P42-48OyFor matrix, wherein y is molal quantity, y=168~199, by mixing 0.02~0.11 mole of Eu3+ Or Tb3+Enter In3+Position, obtains.
A kind of RE phosphate phosphor material powder the most according to claim 2, it is characterised in that described phosphate Mg21-28In28-34P42-48OyMatrix belongs to anorthic system, P-1 (No.2) space group.
A kind of RE phosphate phosphor material powder the most according to claim 1, it is characterised in that Mg21-28(In1-xEux)28-34P42-48OyEffective excitation wavelength be positioned at 210~280nm in the range of, for red fluorescence powder.
A kind of RE phosphate phosphor material powder the most according to claim 1, it is characterised in that Mg21-28(In1-xTbx)28-34P42-48OyEffective excitation wavelength be positioned at 210~280nm in the range of, for green emitting phosphor.
6. the preparation method of the RE phosphate phosphor material powder described in any one of claim 1-5, is characterized by: according to chemistry Formula is Mg21-28(In1-xLnx)28-34P42-48OyRequired nonstoichiometric molar ratio weighs MgO, In2O3、Eu2O3Or Tb4O7, and NH4H2PO4, it is placed in beaker, adds strong acid and make dissolution of raw material, after solution clarification, add polyvinyl alcohol and deionized water, heating Stirring is to being evaporated completely, and dried material grinds uniformly;At 1100-1300 DEG C, carry out first stage sintering, be cooled to room temperature, Grind, under 1100-1300 DEG C of temperature conditions, then carry out second stage sintering, grind after cooling and obtain end product.
Novel phosphoric acid salt base fluorescent powder the most according to claim 6, it is characterised in that the heating rate of first stage sintering It is 3~7 DEG C/min.
Novel phosphoric acid salt base fluorescent powder the most according to claim 6, it is characterised in that the heating rate of second stage sintering It is 3~7 DEG C/min.
Novel phosphoric acid salt base fluorescent powder the most according to claim 6, it is characterised in that the temperature retention time of first stage sintering 10~20h.
Novel phosphoric acid salt base fluorescent powder the most according to claim 6, it is characterised in that during the insulation that second stage sinters Between 10~20h.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111440612A (en) * 2019-01-16 2020-07-24 中南大学 Barium-indium phosphate fluorescent matrix material and preparation method and application thereof

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