CN109423276A - A kind of Mn of efficient stable4+Doped fluoride luminescent material and preparation method thereof - Google Patents
A kind of Mn of efficient stable4+Doped fluoride luminescent material and preparation method thereof Download PDFInfo
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- CN109423276A CN109423276A CN201710791365.4A CN201710791365A CN109423276A CN 109423276 A CN109423276 A CN 109423276A CN 201710791365 A CN201710791365 A CN 201710791365A CN 109423276 A CN109423276 A CN 109423276A
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/61—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing fluorine, chlorine, bromine, iodine or unspecified halogen elements
- C09K11/615—Halogenides
- C09K11/616—Halogenides with alkali or alkaline earth metals
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/674—Halogenides
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Abstract
The invention discloses a kind of modification Mn of efficient stable4+Doped fluoride luminescent material and preparation method thereof, the preparation method can efficiently synthesize A within the temperature range of 0-120 DEG C2MF6The A of compound cladding2MF6:Mn4+It is fluorinated matter fluorescent powder, avoids Mn4+It directly contacts and degrades with external environment, there is high-temperature stability and good anti humility performance, and further improve the luminous efficiency of fluorescent powder.This method preparation temperature is low, the time is short, technique is easy to control, is suitble to industrial-scale preparation.
Description
Technical field
The present invention relates to rare earth luminescent materials and lighting display technology field, more particularly, to a kind of Mn of efficient stable4+
Doped fluoride luminescent material and preparation method thereof.
Background technique
White light LEDs are as a kind of novel solid state light emitter, and compared with the light sources such as traditional incandescent lamp and fluorescent lamp, it has
It the advantages that environmentally friendly, energy saving, efficient, response is fast, is known as after incandescent lamp, fluorescent lamp and the big light source of high-voltage gas discharging light three
Forth generation green light source.In LED light source, the performance of fluorescent powder determine the luminous efficiency of LED, colour rendering index, colour temperature and
The technical indicators such as service life, therefore, fluorescent powder have very important status in white light LEDs, receive significant attention.At present
Most common method is by blue-light LED chip (emission wavelength 440-480nm) and yellow fluorescent powder (such as YAG:Ce or TAG:Ce)
Combine, yellow fluorescent powder launches yellow light after absorbing the blue light that some blue light LED chip issues, and with unabsorbed blue light
It is mixed to form white light.But can only obtain in this way correlated colour temperature (Correlated Color Temperature,
CCT) it is greater than the cool white optical device of 4500K, meanwhile, colour rendering index (Color Rendering Index, CRI) is relatively low, leads to
Often less than 80.It causes to be difficult to obtain low main reason is that the feux rouges composition in common yellow fluorescent powder emission spectrum is insufficient
The white light LED part of colour temperature, warm tones and high color rendering index (CRI), and this is exactly the key that white light LEDs can obtain application indoors.
To realize that this target, an effective method are exactly to add red light fluorescent powder appropriate, booster in white light LED part
The red emission of part.
Mn4+Ion-activated fluoride materials have narrow emission peak, and half-peak breadth is small, is grinding for current red emitting material
Study carefully hot spot.Patent US2009/7497973 discloses Mn4+The A of activation2MF6(A K, Na, Rb etc.；M is Ti, Si, Sn, Ge etc.)
Red light fluorescent powder；Wherein by the way that by dissolution of raw material, in high concentration of hydrofluoric acid, then heating volatilization cocrystallization obtains product；Patent
WO2009/119486, which is disclosed, to be dissolved in metal such as Si in the solution of hydrofluoric acid and potassium permanganate, and reaction obtains fluorination produce
Object；Patent CN102732249A, which is disclosed, reports the first solution by first preparing the fluoride containing metal M and containing A's
The compound of the A of second of solution or solid form, the two is mixed, and is generated precipitating after reacted, is obtained product；These methods
The fluoride luminescent material of preparation all has luminous efficiency height, the good advantage of thermal stability.But these methods all do not overcome fluorine
The shortcomings that compound luminescent material facile hydrolysis, is easy hydrolysis under long-time service or wet environment, is that luminous efficiency reduces even mistake
Effect.Patent US2007/0125984 A1, which is reported, coats one layer of inorganic material (such as TiO on fluoride surface2、Al2O3、SiO2)
Protective film avoids Mn4+It is directly contacted with water and generates hydrolysis；Patent CN106479485 A, which is equally disclosed, is reported in fluorescent powder
Particle surface coats one layer of potassium silicate-sodium cellulose glycolate-polyethylene glycol mixture, improves the high temperature and humidity resistance of fluorescent powder
Energy；The humidity-proof ability that these open methods introduced can effectively improve fluorescent powder reduces the hair of material but then
Light efficiency.
Summary of the invention
In order to solve the deficiencies in the prior art, the purpose of the present invention is to provide a kind of Mn of efficient stable4+Doping fluorination
Object luminescent material and preparation method thereof, to solve the disadvantage of fluoride luminescent material high temperature resistant moisture resistance properties deficiency, while can
The effective luminous efficiency for improving fluorescent powder.With preparation process, simple, raw material sources are extensively and hydrofluoric acid consumes for this method
Small feature is measured, industrialization large scale preparation is suitable for.
The purpose of the present invention is achieved through the following technical solutions:
A kind of modified Mn4+The preparation method of doped fluoride luminescent material, the luminescent material are surface by A2MF6Cladding
Mn4+Doped fluoride A2MF6:Mn4+；
Wherein, A is selected from alkali metal Li, Na, K, Rb, one of Cs or the combination between them；
M is selected from Ti, Si, Ge, Sn, one of Zr or the combination between them；
Mn4+For luminescent center ion；
It is characterized in that, described method includes following steps:
(1) by A2MF6It is dissolved in HF solution and forms saturated solution；
(2) by saturated solution and A2MF6:Mn4+Luminescent material mixing, stirring is impregnated, and after filtration drying, obtains primary place
A after reason2MF6:Mn4+Powder；
(3) A that will be obtained after the saturated solution of step (1) and step (2) filtration drying2MF6:Mn4+Powder mixing, again
Stirring is impregnated, the A after filtration drying, after obtaining secondary treatment2MF6:Mn4+Powder repeats the above steps, and is prepared described
Modified Mn4+Doped fluoride luminescent material.
According to the present invention, in step (3), the number for repeating step is 1-6 times, preferably 2-5 times.
According to the present invention, the M is preferably Si and/or Ti.
According to the present invention, the alkali metal A is preferably Na and/or K.
According to the present invention, the Mn4+Doped fluoride A2MF6:Mn4+Selected from K2SiF6:Mn4+、K2TiF6:Mn4+、K2SnF6:
Mn4+、Cs2SiF6:Mn4+、Rb2GeF6:Mn4+、Rb2SiF6:Mn4+、Na2TiF6:Mn4+、Na2SiF6:Mn4+、Na2ZrF6:Mn4+、
K2GeF6:Mn4+, preferably Na2TiF6:Mn4+、Na2SiF6:Mn4+、K2TiF6:Mn4+、K2SiF6:Mn4+。
According to the present invention, the A2MF6For corresponding matrix compounds.
According to the present invention, the A2MF6Selected from K2SiF6、K2TiF6、K2SnF6、Cs2SiF6、Rb2GeF6、Rb2SiF6、
Na2TiF6、Na2SiF6、Na2ZrF6、K2GeF6, preferably Na2TiF6、Na2SiF6、K2TiF6、K2SiF6。
According to the present invention, in step (1), the preferred 20-50% of the mass percent of the hydrofluoric acid.
According to the present invention, in step (1), the saturated solution is preferably formed at 20 DEG C -120 DEG C.
According to the present invention, in step (2) and (3), the temperature that the stirring is impregnated is 0-120 DEG C, preferably 20-50 DEG C.
According to the present invention, in step (2) and (3), stirring immersion can be to be carried out under heat-retaining condition, can also be
Carried out under the conditions of slow cooling, it is preferable that the slow cooling rate be 0.1 DEG C/min-10 DEG C/min, preferably 0.5 DEG C/
min-5℃/min。
According to the present invention, in step (2) and (3), the time that the stirring is impregnated is 2min-2h, preferably 5min-1h.
According to the present invention, in step (2) and (3), the A2MF6And A2MF6:Mn4+Molar ratio be 1-5:1.
According to the present invention, in step (2) and (3), product after filtering can be further with organic solvent such as dehydrated alcohol
Or acetone is washed, and to remove the acid solution of surface residual, and is dried.
In the present invention, A can be made through the method2MF6:Mn4+The Mn on surface4+With saturation A2MF6M in solution4+Realize from
Son exchange, eliminates A2MF6:Mn4+The Mn on surface4+, A is formed in phosphor surface2MF6Compound protective layer, while reducing activation
Ion Mn4+In A2MF6:Mn4+The defect that phosphor surface is formed.
In the present invention, when the stirring soaking process carries out under heat-retaining condition, powder sample after filtration drying,
Superficial layer is A2MF6The A of compound2MF6:Mn4+It is fluorinated matter fluorescent powder, fluorescent powder grain size does not change, during being somebody's turn to do,
A2MF6:Mn4+It is fluorinated the Mn on matter fluorescent powder surface layer4+Ion-exchange reactions, therefore, the fluorescent powder occurs with the M ion in solution
The size of grain does not change.
Powder in the present invention, when the stirring soaking process carries out under the conditions of slow cooling, after filtration drying
Sample, superficial layer A2MF6The A of compound2MF6:Mn4+It is fluorinated matter fluorescent powder, fluorescent powder grain size increases, during being somebody's turn to do,
A2MF6:Mn4+Crystallization cladding, the A in ie in solution mainly occur for fluorination matter fluorescent powder2MF6Compound is precipitated with the variation of temperature
And it is coated on A2MF6:Mn4+It is fluorinated matter fluorescent powder surface layer, therefore, which increases.
The present invention also provides a kind of modified Mn4+Doped fluoride luminescent material is prepared using the above method.
Beneficial effects of the present invention:
The present invention provides a kind of modification Mn of efficient stable4+Doped fluoride luminescent material and preparation method thereof, it is described
Preparation method can efficiently synthesize A within the temperature range of 0-120 DEG C2MF6The A of compound cladding2MF6:Mn4+Fluoride fluorescence
Powder avoids Mn4+It directly contacts and degrades with external environment, there is high-temperature stability and good anti humility performance, and into one
Step improves the luminous efficiency of fluorescent powder.This method preparation temperature is low, the time is short, technique is easy to control, is suitble to industrial-scale system
It is standby.
Detailed description of the invention
K in Fig. 1 embodiment of the present invention 22TiF6:Mn4+The XRD diffracting spectrum of fluorescent powder.
K in Fig. 2 embodiment of the present invention 22TiF6:Mn4+The excitation spectrum and emission spectrum of fluorescent powder.
K in Fig. 3 embodiment of the present invention 62SiF6:Mn4+The XRD diffracting spectrum of fluorescent powder.
K in Fig. 4 embodiment of the present invention 62SiF6:Mn4+The excitation spectrum and emission spectrum of fluorescent powder.
Specific embodiment
The present invention is further detailed below with reference to embodiment.But skilled in the art realises that following implementations
Example is not limiting the scope of the invention, any improvements and changes made on the basis of the present invention, all of the invention
Within protection scope.
Embodiment 1:K2TiF6:Mn4+The preparation of fluorescent powder
By 0.4000g K2MnF6It is dissolved in 6mL hydrofluoric acid (49wt.%) solution, stirring obtains orange-yellow transparent for 5 minutes
Solution, then by 5.1850g K2TiF6Powder is added in solution, continue at room temperature stirring 30 minutes, stop stir and with filter
Paper filtering, then cleaned with acetone, any remaining HF that goes out obtains K by drying2TiF6:Mn4+Powder.Pass through
FLS980 type (Edinburgh Instrument) Fluorescence Spectrometer measures the excitation and emission spectra and fluorescence volume of product
Sub- yield and absorption efficiency.
Embodiment 2: modified K2TiF6:Mn4+The preparation of fluorescent powder
By the way that K is added into 10ml 49%HF solution2TiF6Compound, (about 1.7000g, room until no longer dissolving
Under temperature), filter undissolved K2TiF6, obtain K2TiF6Saturated solution in 49%HF solution.Then the saturated solution is added
Enter to equipped with the K obtained in embodiment 12TiF6:Mn4+In the container of fluorescent powder, it is continuously stirred at room temperature 30min.With laggard
Row vacuum filtration；It repeats above-mentioned stirring soaking step 2 times, after finally filtering for several times with acetone washing, residual HF is removed, by 70
After DEG C dry 2h, fluorescent powder is obtained.It is hexagonal phase K that X-ray powder diffraction, which shows product still,2TiF6Structure (Fig. 1)；Pass through
FLS980 type (Edinburgh Instrument) Fluorescence Spectrometer measures the excitation and emission spectra and interior fluorescence of product
Quantum yield, Fig. 2 are its excitation and emission spectra, and table 1 gives important materialization and the optical performance parameter of prepared fluorescent powder,
Including Mn4+Doping concentration, prepare the fluorescence quantum yield and absorption efficiency of raw material proportioning and sample.
Embodiment 3: modified K2TiF6:Mn4+The preparation of fluorescent powder
By the way that K is added into 10ml 49%HF solution2TiF6Compound, solution are heated to 70 DEG C and are stirred continuously until not
Until redissolution (about 2.3000g), undissolved K is filtered2TiF6, obtain K2TiF6Saturation at 70 DEG C in 49%HF solution
Solution.Then the saturated solution is added to equipped with the K obtained in embodiment 12TiF6:Mn4+In the container of fluorescent powder, with 0.5
DEG C/the cooling rate slow cooling of min, and continue stirring until room temperature.It is then filtered by vacuum, for several times with acetone washing, is removed
Go residual HF, after 70 DEG C of dry 2h, obtain fluorescent powder.Table 1 gives important materialization and the optics of prepared fluorescent powder
Performance parameter, including Mn4+Doping concentration, prepare the fluorescence quantum yield and absorption efficiency of raw material proportioning and sample.
Embodiment 4: stability test
The fluorescent powder sample that embodiment 1, embodiment 2 and embodiment 3 prepare is impregnated into certain time in water respectively,
Test the comparison of its luminous intensity values.Example 1 respectively, 3 fluorescent powder sample 0.5000g of embodiment 2 and embodiment measure 1ml
Distilled water is added in sample, impregnates 10min respectively, after filtration drying, luminous intensity such as 1 institute of table after being impregnated in the water surveyed respectively
Show.
1 K of table2TiF6:Mn4+Fluorescence property compares fluorescent powder before and after the processing
The quantum yield of fluorescent powder is improved it can be seen from table after modification, it is often more important that improve fluorescence
The moisture-resistant stability of powder, luminous intensity decaying is few after impregnating in water.
Embodiment 5:K2SiF6:Mn4+The preparation of fluorescent powder
By 0.3250g K2MnF6It is dissolved in 4mL hydrofluoric acid (49%) solution, stirring obtains orange-yellow transparent molten for 5 minutes
Liquid, then by 5.5000g K2SiF6Powder is added in solution, and continues stirring 3 hours at room temperature, uses filter after stopping stirring
K is obtained by filtration in paper2SiF6:Mn4+Powder, X-ray powder diffraction show that product has cubic phase K2SiF6Structure is excited in blue light
Under, which issues bright feux rouges.
Embodiment 6: modified K2SiF6:Mn4+The preparation of fluorescent powder
By the way that K is added into 10ml 49%HF solution2SiF6Compound, (about 0.1750g, room until no longer dissolving
Under temperature), filter undissolved K2SiF6, obtain K2SiF6Saturated solution in 49%HF solution.It will then be obtained in embodiment 5
The K obtained2SiF6:Mn4+Fluorescent powder is added in the saturated solution, is continuously stirred at room temperature 30min.Then carry out vacuum pumping
Filter repeats above-mentioned stirring soaking step 2 times, after finally filtering for several times with acetone washing, residual HF is removed, by 70 DEG C of dry 2h
Afterwards, fluorescent powder is obtained.It is hexagonal phase K that X-ray powder diffraction, which shows product still,2SiF6Structure (Fig. 3)；Pass through FLS980 type
(Edinburgh Instrument) Fluorescence Spectrometer measures the excitation and emission spectra and interior fluorescence quantum yield of product,
Fig. 4 is its excitation and emission spectra, and table 2 gives important materialization and the optical performance parameter of prepared fluorescent powder, including Mn4+'s
Doping concentration prepares the fluorescence quantum yield and absorption efficiency of raw material proportioning and sample.
Embodiment 7: modified K2SiF6:Mn4+The preparation of fluorescent powder
By the way that K is added into 10ml 49%HF solution2SiF6Compound, solution are heated to 70 DEG C and are stirred continuously until not
Until redissolution (about 0.2200g), undissolved K is filtered2SiF6, obtain K2SiF6Saturation at 70 DEG C in 49%HF solution
Solution.Then the saturated solution is added to equipped with the K obtained in embodiment 52SiF6:Mn4+In the container of fluorescent powder, with 0.5
DEG C/the cooling rate slow cooling of min, and continue stirring until room temperature.It is then filtered by vacuum, for several times with acetone washing, is removed
Go residual HF, after 70 DEG C of dry 2h, obtain fluorescent powder.Table 2 gives important materialization and the optics of prepared fluorescent powder
Performance parameter, including Mn4+Doping concentration, prepare the fluorescence quantum yield and absorption efficiency of raw material proportioning and sample.
Embodiment 8: stability test
The fluorescent powder sample that embodiment 5, embodiment 6 and embodiment 7 prepare is impregnated into certain time in water respectively,
Test the comparison of its luminous intensity values.Example 5 respectively, 7 fluorescent powder sample 0.5000g of embodiment 6 and embodiment measure 1ml
Distilled water is added in sample, impregnates 10min respectively, after filtration drying, luminous intensity such as 2 institute of table after being impregnated in the water surveyed respectively
Show.
2 K of table2SiF6:Mn4+Fluorescence property compares fluorescent powder before and after the processing
The quantum yield of fluorescent powder is improved it can be seen from table after modification, it is often more important that improve fluorescence
The moisture-resistant stability of powder, luminous intensity decaying is few after impregnating in water.
More than, embodiments of the present invention are illustrated.But the present invention is not limited to above embodiment.It is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in guarantor of the invention
Within the scope of shield.
Claims (10)
1. a kind of modified Mn4+Doped fluoride luminescent material and preparation method thereof, the luminescent material are surface by A2MF6Cladding
Mn4+Doped fluoride A2MF6:Mn4+；
Wherein, A is selected from alkali metal Li, Na, K, Rb, one of Cs or the combination between them；
M is selected from Ti, Si, Ge, Sn, one of Zr or the combination between them；
Mn4+For luminescent center ion；
It is characterized in that, described method includes following steps:
(1) by A2MF6It is dissolved in HF solution and forms saturated solution；
(2) by saturated solution and A2MF6:Mn4+Luminescent material mixing, stirring is impregnated, after filtration drying, after obtaining single treatment
A2MF6:Mn4+Powder；
(3) A that will be obtained after the saturated solution of step (1) and step (2) filtration drying2MF6:Mn4+Powder mixing, is again stirring for
It impregnates, the A after filtration drying, after obtaining secondary treatment2MF6:Mn4+Powder repeats the above steps, and the modification is prepared
Mn4+Doped fluoride luminescent material.
2. preparation method according to claim 1, which is characterized in that in step (3), the number for repeating step is 1-6 times,
It is preferred that 2-5 times.
3. preparation method according to claim 1 or 2, which is characterized in that the M is Si and/or Ti.
Preferably, the alkali metal A is Na and/or K.
4. preparation method according to any one of claim 1-3, which is characterized in that the Mn4+Doped fluoride A2MF6:
Mn4+Selected from K2SiF6:Mn4+、K2TiF6:Mn4+、K2SnF6:Mn4+、Cs2SiF6:Mn4+、Rb2GeF6:Mn4+、Rb2SiF6:Mn4+、
Na2TiF6:Mn4+、Na2SiF6:Mn4+、Na2ZrF6:Mn4+、K2GeF6:Mn4+, preferably Na2TiF6:Mn4+、Na2SiF6:Mn4+、
K2TiF6:Mn4+、K2SiF6:Mn4+。
5. preparation method described in any one of -4 according to claim 1, which is characterized in that the A2MF6For corresponding matrix
Compound.
Preferably, the A2MF6Selected from K2SiF6、K2TiF6、K2SnF6、Cs2SiF6、Rb2GeF6、Rb2SiF6、Na2TiF6、
Na2SiF6、Na2ZrF6、K2GeF6, preferably Na2TiF6、Na2SiF6、K2TiF6、K2SiF6。
6. preparation method according to any one of claims 1-5, which is characterized in that in step (1), the hydrofluoric acid
The preferred 20-50% of mass percent.
Preferably, in step (1), the saturated solution is preferably formed at 20 DEG C -120 DEG C.
7. preparation method according to claim 1 to 6, which is characterized in that described to stir in step (2) and (3)
The temperature for mixing immersion is 0-120 DEG C, preferably 20-50 DEG C.
Preferably, in step (2) and (3), the stirring immersion can be to be carried out under heat-retaining condition, can also be in slow cooling
Under the conditions of carry out, it is preferable that the slow cooling rate be 0.1 DEG C/min-10 DEG C/min, also preferably 0.5 DEG C/min-5 DEG C/
min。
Preferably, in step (2) and (3), the time that the stirring is impregnated is 2min-2h, preferably 5min-1h.
8. preparation method described in any one of -7 according to claim 1, which is characterized in that described in step (2) and (3)
A2MF6And A2MF6:Mn4+Molar ratio be 1-5:1.
9. preparation method according to claim 1 to 8, which is characterized in that in step (2) and (3), through filtering
Product afterwards can be washed further with organic solvent such as dehydrated alcohol or acetone, to remove the acid solution of surface residual, be gone forward side by side
Row drying.
10. a kind of modified Mn4+Doped fluoride luminescent material is using method system of any of claims 1-9
For what is obtained.
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| CN111471456A (en) * | 2020-04-11 | 2020-07-31 | 厦门市钛科创科技有限公司 | Fluoride red fluorescent powder and luminescent device based on same |
| CN114276804A (en) * | 2020-09-28 | 2022-04-05 | 厦门稀土材料研究所 | Nano-submicron fluoride luminescent material, preparation method and luminescent device |
| CN113337279A (en) * | 2021-04-30 | 2021-09-03 | 湖南师范大学 | Fluoride fluorescent powder and preparation method thereof |
| JP7364927B2 (en) | 2021-10-13 | 2023-10-19 | 日亜化学工業株式会社 | Fluoride phosphor, its manufacturing method and light emitting device |
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