CN105754596B - A kind of rear-earth-doped fluozirconate luminescent material and preparation method thereof - Google Patents
A kind of rear-earth-doped fluozirconate luminescent material and preparation method thereof Download PDFInfo
- Publication number
- CN105754596B CN105754596B CN201610193188.5A CN201610193188A CN105754596B CN 105754596 B CN105754596 B CN 105754596B CN 201610193188 A CN201610193188 A CN 201610193188A CN 105754596 B CN105754596 B CN 105754596B
- Authority
- CN
- China
- Prior art keywords
- earth
- doped
- luminescent material
- fluozirconate
- preparation
- 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.)
- Active
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
- C09K11/7715—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing cerium
- C09K11/7719—Halogenides
- C09K11/772—Halogenides with alkali or alkaline earth metals
-
- 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
- C09K11/7704—Halogenides
- C09K11/7705—Halogenides with alkali or alkaline earth metals
-
- 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
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7732—Halogenides
- C09K11/7733—Halogenides with alkali or alkaline earth metals
-
- 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
- C09K11/7747—Halogenides
- C09K11/7748—Halogenides with alkali or alkaline earth metals
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 rear-earth-doped fluozirconate luminescent material and preparation method thereof.The chemical composition of the material is Sr(1‐x)ZrF6:xRE3+, wherein RE=Eu, Tb, Ce or Dy, 0.5%≤x≤7.0%；Its preparation method is as follows：By solid fluorinated strontium and rare earth oxide, stoichiometrically precise is put into inner liner of reaction kettle, adds fluorine zirconic acid and deionized water, stirring, fills this blend into reactor, reacted at 120~220 DEG C, obtains the bar-shaped luminescent material of micron of complete crystallization.Material phonon energy is low, and the centre of luminescence is radiationless, and relaxation rate is low, and luminous efficiency is high.Material granule disperses, and does not reunite, and is advantageous to apply pipe application.Material crystalline degree is high, and matrix is stable, is applied in wet environment without hydrolyzing.The material can be used for electricity-saving lamp and high-pressure sodium lamp, and preparation technology is simple, low for equipment requirements.
Description
Technical field
The present invention relates to inoganic solids luminescent material, more particularly to it is a kind of available for electricity-saving lamp and high-pressure sodium lamp with fluorine
Strontium zirconate is luminescent material of matrix and preparation method thereof.More particularly to one kind using fluorine zirconic acid strontium as matrix, with Eu3+(or Tb3+、
Ce3+With Dy3+) be active ions luminescent material, its luminous efficiency is suitable with the Commercial optical powder synthesized with high temperature solid-state method.
Background technology
Electricity-saving lamp (254nm) and high-pressure sodium lamp (365nm) are as traditional photo light source, with its high colour developing, high efficiency, durable
The features such as, it is still widely used in the production and living of people, is the leading products in current illumination market.To obtain white light, need
Three kinds are glowed respectively, green glow and blue light and has the luminescent material absorbed by force in ultra-violet (UV) band, uniformly mixing by a certain percentage,
Launch the fluorescence of red, green and blueness simultaneously and form white light.The luminescent material quilt of visible ray can be converted ultraviolet light into
It is widely used in electricity-saving lamp (254nm) and high-pressure sodium lamp (365nm), such as three primary colors fluorescent powder：Rouge and powder Y2O3:Eu3+
[J.Dhanaraj, R.Jagannathan, T.R.N.Kutty, C.H.Lu, J.Phys.Chem.B, 2001,105,11098-
11105.] and YVO4:Eu3+[M.Yu, J.Lin, J.Fang, Chem.Mater., 2005,17,1783-1791.], green powder
LaPO4:Ce3+,Tb3+[Mei Yang,H.P.You,K.Liu,Y.H.Zheng,N.Guo,H.J.Zhang,Inorg.Chem.,
2010,49 (11), 4996-5002.] and Zn2SiO4:Mn2+[C.Bertail,S.Maron,V.Buissette,
T.L.Mercier, T.Gacoin, J.P.Boilot, Chem.Mater., 2011,23,2961-2967.], blue powder
BaMgAl10O17:Eu2+[H.Y.Ni,H.B.Liang,Q.Su,Y.Tao,Y.Huang,Z.H.Gao,J.Am.Ceram.Soc.,
2012,95,3197-3201.] etc., it is industrial that such fluorescent material is typically synthesized using high temperature solid-state method, first, equipment is more ripe,
Second, the product crystallinity that high temperature solid-state method obtains is high, so that luminous efficiency is high.Red, green, blue powder is mixed by a certain percentage,
In the case where the common excitation wavelength (being normally at ultra-violet (UV) band) of three kinds of powder excites, white light is produced.But needed for high temperature solid-state method synthesis
Want sintering temperature to be generally greater than 1000 DEG C and need to grind repeatedly with repeatedly sintering, product is reunited seriously, crushing process ghost image
Ring product luminescent properties.
In recent years, it has been found that Mn4+Mix fluosilicate such as K2SiF6[J.H.Oh,H,Kang,Y.J.Eo,H.K.Park,
Y.G.Do,J.Mater.Chem.C,2015,3,607‐615.]、BaSiF6[X.Y.Jiang,Y.X.Pan,S.M.Huang,
X.A.Chen, J.G.Wang, G.K.Liu, J.Mater.Chem.C.2014,2 (13), 2301-2306.] and fluotitanate is such as
BaTiF6[X.Y.Jiang,Z.Chen,S.M.Huang,J.G.Wang,Y.X.Pan,Dalton Trans.2014,43,9414‐
When 9418.], feux rouges, Mn therein can be launched4+Substitute Si4+Or Ti4+Position, the position without substituting alkaline earth or alkali metal ion
Put, but Mn4+In the matrix SrZrF of the present invention6In do not light, not yet synthesize so far successfully, possible Mn4+SrZrF is not entered6In
Zr4+Position.
The content of the invention
It is an object of the invention to provide a kind of rear-earth-doped fluozirconate luminescent material, materials synthesis temperature is low, system
Standby technique is simple, and product particle is uniform, good dispersion, and luminous efficiency is high.
The purpose of the present invention is achieved through the following technical solutions：
A kind of rear-earth-doped fluozirconate luminescent material, its chemical composition are Sr(1‐x)ZrF6:xRE3+, wherein RE=Eu,
Tb, Ce or Dy, 0.5%≤x≤7.0%, can efficient transmission visible ray after material absorbs ultraviolet light.
The excitation spectrum of rear-earth-doped fluozirconate luminescent material is located at 200~400nm, mixes Eu3+When, glow；Mix
Tb3+When, green light；Mix Ce3+When, blue light-emitting；Mix Dy3+When, emit white light.
The preparation method of described rear-earth-doped fluozirconate luminescent material：Solid fluorinated strontium is pressed with rare earth oxide
Stoichiometric proportion precise is put into inner liner of reaction kettle, then adds fluorine zirconic acid and deionized water, stirs, mixture is filled
Enter in reactor, 120~220 DEG C are reacted 4~8 hours, and reaction finishes, cooling, and the micron that complete crystallization is produced after suction filtration is bar-shaped
Rear-earth-doped fluozirconate luminescent material.
Preferably, the inner liner of reaction kettle is polytetrafluoroethyllining lining.
Preferably, the reactor is stainless steel cauldron.
Preferably, the temperature for controlling stainless steel cauldron to react is 150~200 DEG C.
Preferably, the time for controlling stainless steel cauldron to react is 5~7 hours.
Preferably, the time of the stirring is 10~20 minutes.
Preparation process of the present invention is one-step synthesis, without sintering.
Relative to prior art, the invention has the advantages that and beneficial effect：Using fluorine zirconic acid strontium as matrix in the present invention
Luminescent material can simultaneously it is near ultraviolet excitated, send visible fluorescence, the business powder phase that fluorescence efficiency synthesizes with high temperature solid-state method
When.Hydrothermal condition synthesizes in next step, and without sintering, synthesis temperature is far below high temperature solid-state method, product particle good crystallinity, easily divides
Dissipate, without needing crushing process.
Brief description of the drawings
Material Sr prepared by Fig. 1 embodiment of the present invention 10.98ZrF6:0.02Eu3+XRD.
Material Sr prepared by Fig. 2 embodiment of the present invention 10.98ZrF6:0.02Eu3+SEM figure.
Material Sr prepared by Fig. 3 embodiment of the present invention 10.98ZrF6:0.02Eu3+Excitation spectrum and emission spectrum.
Material Sr prepared by Fig. 4 embodiment of the present invention 40.99ZrF6:0.01Tb3+Excitation spectrum and emission spectrum.
Material Sr prepared by Fig. 5 embodiment of the present invention 70.97ZrF6:0.03Ce3+Excitation spectrum and emission spectrum.
Material Sr prepared by Fig. 6 embodiment of the present invention 100.96ZrF6:0.04Dy3+Excitation spectrum and emission spectrum.
Embodiment
The invention will be further described with reference to the accompanying drawings and examples, and the scope of protection of present invention is not limited to
In the scope of embodiment statement.
Embodiment 1
Sr in molar ratio：[ZrF6]：Eu=0.98：1：0.02, with the solid fluorinated strontium SrF of electronic balance precise2(point
Analyse pure) and europium oxide Eu2O3(4N), ptfe autoclave liner is put into, fluorine zirconic acid addition is accurately measured with pipette, then
Add deionized water reaction system cumulative volume is reached 40mL (account for reactor inner product 80%), magnetic agitation 15 minutes, will be equipped with mixed
The liner of compound is placed in closed stainless steel cauldron.Baking oven is put into reactor transfer, 12 hours are incubated at 180 DEG C.React
Finish, cooling, naturally dry after suction filtration, product population is about 3 grams.Product sends bright red fluorescence under near ultraviolet irradiation.
Fig. 1 XRD shows the SrZrF that product is pure phase6, trace doped Eu3+Substantially do not change crystal structure.Fig. 2 SEM represents production
Product Sr0.98ZrF6:0.02Eu3+Particle is bar-shaped in micron, well dispersed, and particle size distribution is concentrated, and is advantageous to apply pipe application, this
Performance is better than the luminescent material synthesized in the market with high temperature solid-state method.Fig. 3 shows Sr0.98ZrF6:0.02Eu3+Exciting light
Spectrum and emission spectrum, in terms of excitation spectrum, the material has very strong absorption near ultraviolet band, with electricity-saving lamp, the ripple of high-pressure sodium lamp
Long matching, available for electricity-saving lamp and high-pressure sodium lamp material, its emission spectrum is located at red light region, therefore the material can be applied to save
Can lamp, the tricolor powder of high-pressure sodium lamp.
In the present invention, the product XRD of other embodiments show be pure phase SrZrF6, SEM figures are similar to Fig. 2, no
Illustrate one by one.
Embodiment 2
Sr in molar ratio：[ZrF6]：Eu=0.995：1：0.005, with the solid fluorinated strontium SrF of electronic balance precise2
(analysis is pure) and europium oxide Eu2O3(4N), ptfe autoclave liner is put into, fluorine zirconic acid addition is accurately measured with pipette,
Again plus deionized water makes reaction system cumulative volume reach 40mL (account for reactor inner product 80%), magnetic agitation 10 minutes, will be equipped with
The liner of mixture is placed in closed stainless steel cauldron.Baking oven is put into reactor transfer, 4 hours are incubated at 220 DEG C.React
Finish, cooling, naturally dry after suction filtration, product population is about 3 grams.Product sends bright red fluorescence under near ultraviolet irradiation.
Its excitation spectrum is substantially similar to emission spectrum to Fig. 3.
Embodiment 3
Sr in molar ratio：[ZrF6]：Eu=0.93：1：0.07, with the solid fluorinated strontium SrF of electronic balance precise2(point
Analyse pure) and europium oxide Eu2O3(4N), ptfe autoclave liner is put into, fluorine zirconic acid addition is accurately measured with pipette, then
Add deionized water reaction system cumulative volume is reached 40mL (account for reactor inner product 80%), magnetic agitation 10 minutes, will be equipped with mixed
The liner of compound is placed in closed stainless steel cauldron.Baking oven is put into reactor transfer, 4 hours are incubated at 220 DEG C.React
Finish, cooling, naturally dry after suction filtration, product population is about 3 grams.Product sends bright red fluorescence under near ultraviolet irradiation.
Its excitation spectrum is substantially similar to emission spectrum to Fig. 3.
Embodiment 4
Sr in molar ratio：[ZrF6]：Tb=0.99：1：0.01, with the solid fluorinated strontium SrF of electronic balance precise2(point
Analyse pure) and terbium oxide Tb4O7(4N), ptfe autoclave liner is put into, fluorine zirconic acid addition is accurately measured with pipette, then
Add deionized water reaction system cumulative volume is reached 40mL (account for reactor inner product 80%), magnetic agitation 15 minutes, will be equipped with mixed
The liner of compound is placed in closed stainless steel cauldron.Baking oven is put into reactor transfer, 18 hours are incubated at 140 DEG C.React
Finish, cooling, naturally dry after suction filtration, product population is about 3 grams.Product sends bright green fluorescence under near ultraviolet irradiation.
Fig. 4 excitation spectrum has very strong absorption near ultraviolet band with emission spectrum display material, and its emission spectrum is located at green wavelength,
It is Tb3+Characteristic emission.
Embodiment 5
Sr in molar ratio：[ZrF6]：Tb=0.995：1：0.005, with the solid fluorinated strontium SrF of electronic balance precise2
(analysis is pure) and terbium oxide Tb4O7(4N), ptfe autoclave liner is put into, fluorine zirconic acid addition is accurately measured with pipette,
Again plus deionized water makes reaction system cumulative volume reach 40mL (account for reactor inner product 80%), magnetic agitation 10 minutes, will be equipped with
The liner of mixture is placed in closed stainless steel cauldron.Baking oven is put into reactor transfer, 4 hours are incubated at 220 DEG C.React
Finish, cooling, naturally dry after suction filtration, product population is about 3 grams.Product sends bright green fluorescence under near ultraviolet irradiation.
The excitation spectrum of material is similar in embodiment 4 to emission spectrum, there is very strong absorption near ultraviolet band, its emission spectrum position
It is Tb in green wavelength3+Characteristic emission.
Embodiment 6
Sr in molar ratio：[ZrF6]：Tb=0.93：1：0.07, with the solid fluorinated strontium SrF of electronic balance precise2(point
Analyse pure) and terbium oxide Tb4O7(4N), ptfe autoclave liner is put into, fluorine zirconic acid addition is accurately measured with pipette, then
Add deionized water reaction system cumulative volume is reached 40mL (account for reactor inner product 80%), magnetic agitation 10 minutes, will be equipped with mixed
The liner of compound is placed in closed stainless steel cauldron.Baking oven is put into reactor transfer, 24 hours are incubated at 120 DEG C.React
Finish, cooling, naturally dry after suction filtration, product population is about 3 grams.Product sends bright green fluorescence under near ultraviolet irradiation.
The excitation spectrum of material is similar in embodiment 4 to emission spectrum, there is very strong absorption near ultraviolet band, its emission spectrum position
It is Tb in green wavelength3+Characteristic emission.
Embodiment 7
Sr in molar ratio：[ZrF6]：Ce=0.97：1：0.03, with the solid fluorinated strontium SrF of electronic balance precise2(point
Analyse pure) and cerium oxide CeO2(4N), ptfe autoclave liner is put into, fluorine zirconic acid addition is accurately measured with pipette, then
Add deionized water reaction system cumulative volume is reached 40mL (account for reactor inner product 80%), magnetic agitation 15 minutes, will be equipped with mixed
The liner of compound is placed in closed stainless steel cauldron.Baking oven is put into reactor transfer, 18 hours are incubated at 140 DEG C.React
Finish, cooling, naturally dry after suction filtration, product population is about 3 grams.Product sends bright blueness under short wavelength UV light irradiation
Fluorescence.Fig. 5 excitation spectrum has very strong absorption near ultraviolet band with emission spectrum display material, and its emission spectrum is located at blue light
Region, it is Ce3+Characteristic emission.
Embodiment 8
Sr in molar ratio：[ZrF6]：Ce=0.995：1：0.005, with the solid fluorinated strontium SrF of electronic balance precise2
(analysis is pure) and cerium oxide CeO2(4N), ptfe autoclave liner is put into, fluorine zirconic acid addition is accurately measured with pipette,
Again plus deionized water makes reaction system cumulative volume reach 40mL (account for reactor inner product 80%), magnetic agitation 10 minutes, will be equipped with
The liner of mixture is placed in closed stainless steel cauldron.Baking oven is put into reactor transfer, 4 hours are incubated at 220 DEG C.React
Finish, cooling, naturally dry after suction filtration, product population is about 3 grams.Product sends bright blue-fluorescence under ultra violet lamp.
The excitation spectrum of material is similar in embodiment 7 to emission spectrum, there is very strong absorption in short wavelength UV area, its emission spectrum
It is Ce positioned at blue region3+Characteristic emission.
Embodiment 9
Sr in molar ratio：[ZrF6]：Ce=0.93：1：0.07, with the solid fluorinated strontium SrF of electronic balance precise2(point
Analyse pure) and cerium oxide CeO2(4N), ptfe autoclave liner is put into, fluorine zirconic acid addition is accurately measured with pipette, then
Add deionized water reaction system cumulative volume is reached 40mL (account for reactor inner product 80%), magnetic agitation 20 minutes, will be equipped with mixed
The liner of compound is placed in closed stainless steel cauldron.Baking oven is put into reactor transfer, 24 hours are incubated at 120 DEG C.React
Finish, cooling, naturally dry after suction filtration, product population is about 3 grams.Product sends bright blue-fluorescence under ultra violet lamp.
The excitation spectrum of material is similar in embodiment 7 to emission spectrum, there is very strong absorption in short wavelength UV area, its emission spectrum
It is Ce positioned at blue region3+Characteristic emission.
Embodiment 10
Sr in molar ratio：[ZrF6]：Dy=0.96：1：0.04, with the solid fluorinated strontium SrF of electronic balance precise2(point
Analyse pure) and dysprosia Dy2O3(4N), ptfe autoclave liner is put into, fluorine zirconic acid addition is accurately measured with pipette, then
Add deionized water reaction system cumulative volume is reached 40mL (account for reactor inner product 80%), magnetic agitation 15 minutes, will be equipped with mixed
The liner of compound is placed in closed stainless steel cauldron.Baking oven is put into reactor transfer, 12 hours are incubated at 180 DEG C.React
Finish, cooling, naturally dry after suction filtration, product population is about 3 grams.Product sends bright white under short wavelength UV light irradiation
Fluorescence.Fig. 6 excitation spectrum has very strong absorption near ultraviolet band with emission spectrum display material, and its emission spectrum is due to blue light
Formed with gold-tinted, be Dy3+Characteristic emission.
Embodiment 11
Sr in molar ratio：[ZrF6]：Dy=0.995：1：0.005, with the solid fluorinated strontium SrF of electronic balance precise2
(analysis is pure) and dysprosia Dy2O3(4N), ptfe autoclave liner is put into, fluorine zirconic acid addition is accurately measured with pipette,
Again plus deionized water makes reaction system cumulative volume reach 40mL (account for reactor inner product 80%), magnetic agitation 10 minutes, will be equipped with
The liner of mixture is placed in closed stainless steel cauldron.Baking oven is put into reactor transfer, 4 hours are incubated at 220 DEG C.React
Finish, cooling, naturally dry after suction filtration, product population is about 3 grams.Product sends bright white fluorescent under ultra violet lamp.
The excitation spectrum of material is similar in embodiment 10 to emission spectrum, there is very strong absorption near ultraviolet band, its emission spectrum
It is Dy because blue light and gold-tinted form3+Characteristic emission.
Embodiment 12
Sr in molar ratio：[ZrF6]：Ce=0.93：1：0.07, with the solid fluorinated strontium SrF of electronic balance precise2(point
Analyse pure) and dysprosia Dy2O3(4N), ptfe autoclave liner is put into, fluorine zirconic acid addition is accurately measured with pipette, then
Add deionized water reaction system cumulative volume is reached 40mL (account for reactor inner product 80%), magnetic agitation 20 minutes, will be equipped with mixed
The liner of compound is placed in closed stainless steel cauldron.Baking oven is put into reactor transfer, 24 hours are incubated at 120 DEG C.React
Finish, cooling, naturally dry after suction filtration, product population is about 3 grams.Product sends bright white fluorescent under ultra violet lamp.
The excitation spectrum of material is similar in embodiment 10 to emission spectrum, there is very strong absorption near ultraviolet band, its emission spectrum
It is Dy because blue light and gold-tinted form3+Characteristic emission.
Luminescent material using fluorine zirconic acid strontium as matrix from above-described embodiment, the present invention can be swashed by near ultraviolet simultaneously
Hair, sends visible fluorescence, fluorescence efficiency is suitable with the business powder that high temperature solid-state method synthesizes.
Hydrothermal condition of the present invention synthesizes in next step, and without sintering, synthesis temperature is far below high temperature solid-state method, product particle knot
Crystalline substance is good, easily scattered, without needing crushing process.
The excitation spectrum of material of the present invention has strong absorption in ultra-violet (UV) band, Wavelength matched with high-pressure sodium lamp with electricity-saving lamp, and
The component particle synthesized under low temperature disperses, size uniform, better than the business powder of high temperature solid-state method synthesis.
Claims (7)
- A kind of 1. preparation method of rear-earth-doped fluozirconate luminescent material, it is characterised in that：By solid fluorinated strontium and rare earth Stoichiometrically precise is put into inner liner of reaction kettle to oxide, then adds fluorine zirconic acid and deionized water, stirs, will Mixture is fitted into reactor, and 120~220 DEG C are reacted 4~8 hours, and reaction finishes, cooling, and complete crystallization is produced after suction filtration The bar-shaped rear-earth-doped fluozirconate luminescent material of micron；The chemical composition of the rear-earth-doped fluozirconate luminescent material is Sr(1‐x)ZrF6:xRE3+, wherein RE=Eu, Tb, Ce Or Dy, 0.5%≤x≤7.0%, after material absorbs ultraviolet light, launch visible ray.
- 2. the preparation method of rear-earth-doped fluozirconate luminescent material according to claim 1, it is characterised in that：It is described Inner liner of reaction kettle is polytetrafluoroethyllining lining.
- 3. the preparation method of rear-earth-doped fluozirconate luminescent material according to claim 1, it is characterised in that：It is described Reactor is stainless steel cauldron.
- 4. the preparation method of rear-earth-doped fluozirconate luminescent material according to claim 3, it is characterised in that：Control The temperature of stainless steel cauldron reaction is 150~200 DEG C.
- 5. the preparation method of rear-earth-doped fluozirconate luminescent material according to claim 4, it is characterised in that：Control The time of stainless steel cauldron reaction is 5~7 hours.
- 6. the preparation method of rear-earth-doped fluozirconate luminescent material according to claim 1, it is characterised in that：It is described The time of stirring is 10~20 minutes.
- 7. the preparation method of rear-earth-doped fluozirconate luminescent material according to claim 1, it is characterised in that：It is described Rear-earth-doped fluozirconate luminescent material emitted light spectrum is located at 200~400nm, mixes Eu3+When, glow；Mix Tb3+When, greening Light；Mix Ce3+When, blue light-emitting；Mix Dy3+When, emit white light.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610193188.5A CN105754596B (en) | 2016-03-30 | 2016-03-30 | A kind of rear-earth-doped fluozirconate luminescent material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610193188.5A CN105754596B (en) | 2016-03-30 | 2016-03-30 | A kind of rear-earth-doped fluozirconate luminescent material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105754596A CN105754596A (en) | 2016-07-13 |
| CN105754596B true CN105754596B (en) | 2018-04-06 |
Family
ID=56345514
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610193188.5A Active CN105754596B (en) | 2016-03-30 | 2016-03-30 | A kind of rear-earth-doped fluozirconate luminescent material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105754596B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033891B (en) * | 2017-06-13 | 2019-07-16 | 温州大学 | A kind of white light LEDs red light material and preparation method thereof based on fluozirconate |
| CN113481005A (en) * | 2021-07-21 | 2021-10-08 | 上海应用技术大学 | Rare earth doped zirconium fluoride cesium-based up-conversion luminescent nano material and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2438012A1 (en) * | 1978-10-03 | 1980-04-30 | Rhone Poulenc Ind | HYDRATED STRONTIUM FLUOSILICATES, ACTIVE AT DIVALENT EUROPE |
| CN105238398A (en) * | 2015-09-28 | 2016-01-13 | 浙江大学 | Rare-earth doped strontium titanate upconversion luminescent nanoparticles and preparation method thereof |
| CN105419795B (en) * | 2015-11-16 | 2018-04-06 | 华南协同创新研究院 | A kind of nano red fluorescent powder of strontium titanates and preparation method for adulterating praseodymium or praseodymium zinc |
-
2016
- 2016-03-30 CN CN201610193188.5A patent/CN105754596B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105754596A (en) | 2016-07-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Yongqing et al. | Properties of red-emitting phosphors Sr2MgSi2O7: Eu3+ prepared by gel-combustion method assisted by microwave | |
| CN115368893B (en) | Sodium gadolinium gallium germanium garnet Dan Jiqing light fluorescent powder and preparation method thereof | |
| CN102660276A (en) | Near ultraviolet stimulated borophosphate white light fluorescent powder and preparation method | |
| CN105754596B (en) | A kind of rear-earth-doped fluozirconate luminescent material and preparation method thereof | |
| CN103555327A (en) | Near ultraviolet excitation double perovskite fluorescent powder for white light LED and preparation method thereof | |
| CN107722982A (en) | Silicon substrate nitrogen oxides hanced cyan fluorescent powder of Fluorescence Increasing and preparation method thereof | |
| CN107365582A (en) | Europium red fluorescence powder and preparation method thereof is mixed suitable for the molybdic acid alkali of white light LEDs | |
| CN100406536C (en) | Novel rare earth three-based colour fluorescence powder and preparation process thereof | |
| CN110437832A (en) | A kind of Eu2+Silicate near-infrared fluorescent powder of doping and preparation method thereof and conversion hysteria LED light emission device | |
| CN108473866A (en) | Fluorophor, light-emitting device, lighting device and image display device | |
| CN109988575A (en) | A kind of Eu3+Ion-activated vanadium phosphorus niobates red fluorescence powder, preparation method and applications | |
| Zou et al. | Structure and luminescent properties of Ca 3 Bi (PO 4) 3: Sm 3+ orange phosphor | |
| CN106590646A (en) | Near-UV excitation blue light fluorescent powder used for white light LED and preparation method thereof | |
| CN104962286A (en) | Garnet-structure multiphase fluorescent material and preparation method thereof | |
| Chen et al. | Luminescence properties of BAM phosphor synthesized by TEA coprecipitation method | |
| EP2540799B1 (en) | Green luminescent material of terbiuim doped gadolinium borate and preparing method thereof | |
| CN104059640B (en) | A kind of borate fluorescent powder substrate and the preparation method of fluorescent material | |
| CN104232081B (en) | A kind of light converting function material and its preparation method and application | |
| CN107312537B (en) | A kind of rare earth-boron Tungstate fluorescent powder and its preparation method and application | |
| Lu et al. | Luminescence characteristics of strontium borate phosphate phosphors | |
| Zhang et al. | Investigation on luminescence of red-emitting Mg3Ca3 (PO4) 4: Ce3+, Mn2+ phosphors | |
| CN104962285A (en) | Submicron Tm3+:beta-Li2TiO3 high purity blue light phosphor and preparation method | |
| CN106554778A (en) | A kind of single-substrate single-doping white luminescent material and preparation method and application | |
| CN102127442B (en) | Zirconium phosphate-based luminescent material as well as preparation method and application thereof | |
| CN102341478A (en) | Oxide luminescent materials activated by trivalent thulium and their preparations |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20160713 Assignee: INSTITUTE OF NEW MATERIALS & INDUSTRIAL TECHNOLOGY, WENZHOU University Assignor: Wenzhou University Contract record no.: X2020330000095 Denomination of invention: A rare earth doped fluorozirconate luminescent material and its preparation method Granted publication date: 20180406 License type: Common License Record date: 20201112 |