CN109401752A - A kind of Mn being stimulated by blue light4+The preparation method of the fluoride luminescent crystal of doping - Google Patents
A kind of Mn being stimulated by blue light4+The preparation method of the fluoride luminescent crystal of doping Download PDFInfo
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- CN109401752A CN109401752A CN201811201923.8A CN201811201923A CN109401752A CN 109401752 A CN109401752 A CN 109401752A CN 201811201923 A CN201811201923 A CN 201811201923A CN 109401752 A CN109401752 A CN 109401752A
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- 239000013078 crystal Substances 0.000 title claims abstract description 49
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 230000005284 excitation Effects 0.000 claims abstract description 13
- 150000002500 ions Chemical class 0.000 claims abstract description 5
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 5
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 26
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- OJOWXSLGSMTXEO-UHFFFAOYSA-H [Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[K+].[K+].[K+].[K+].[K+].[K+] Chemical compound [Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[K+].[K+].[K+].[K+].[K+].[K+] OJOWXSLGSMTXEO-UHFFFAOYSA-H 0.000 claims description 10
- 235000003270 potassium fluoride Nutrition 0.000 claims description 10
- 239000011698 potassium fluoride Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 8
- 239000010955 niobium Substances 0.000 claims description 7
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 7
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 7
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 241001062009 Indigofera Species 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 150000002222 fluorine compounds Chemical group 0.000 abstract 1
- 239000004065 semiconductor Substances 0.000 description 10
- 239000000843 powder Substances 0.000 description 8
- 238000001291 vacuum drying Methods 0.000 description 7
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000000295 emission spectrum Methods 0.000 description 5
- 238000000695 excitation spectrum Methods 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 239000002178 crystalline material Substances 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002109 crystal growth method Methods 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
Classifications
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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
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/674—Halogenides
- C09K11/675—Halogenides with alkali or alkaline earth metals
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The present invention relates to inorganic functional material fields, disclose a kind of Mn that can be stimulated by blue light4+The preparation method of the fluoride luminescent crystal of doping.The Mn of the present invention being stimulated by blue light4+The chemical composition of the fluoride luminescent crystal of doping is K2M1‑xF7:xMn4+；X is corresponding doping Mn4+Ion is with respect to M5+Molar percentage coefficient shared by ion, 0 < x≤0.10；M is Ta or Nb.Fluoride luminescent crystal translucency according to the present invention is good, under blue light excitation, shows a series of narrow emissions, luminous efficiency is high.
Description
Technical field
The present invention relates to the Mn that one kind can be stimulated by blue light4+The preparation method of the fluoride luminescent crystal of doping, it is specific and
Speech, is a kind of blue light GaN base light emitting Mn4+The fluoride luminescent crystal preparation method of doping, belongs to inorganic functional material
Expect preparation field.
Background technique
Current white semiconductor solid-state lighting is widely used in the normal lighting life of people.Traditional semiconductor shines
Mingguang City source is the Y by Yellow light-emitting low temperature3Al5O12:Ce3+The semiconductor chip of powder and blue light-emitting is composed.It is this kind of in order to improve
Suitable powder body material to glow will be added toward contact in white semiconductor illumination light-emitting performance, people.Such as some mix rare earth
The oxynitrides powder and some Mn of ion4+The powder body material of doping.However due in white semiconductor illuminating device system
During work, needs to mix luminescent powder by silica gel, be then applied to semiconductor core on piece, this will lead to such lighting source
Heat dissipation performance is bad, to influence the luminous efficiency and service life of white light LEDs, is less useful in large-power semiconductor device
Application.Compared with powder body material, crystalline material has better heat dissipation performance and light transmission, has on semiconductor lighting
Important application prospect.
In recent years, Mn4+The fluoride red illuminating material of doping causes the extensive concern of people.Such as Mn4+Doping
A2BF6(A Na, K, Rb etc.；B is Ti, Si, Sn, Ge etc.) luminescent properties of powder body material that glow are extensive
Report.K2MF7:Mn4+The luminescent properties of (M is Ta or Nb) also are reported out recently, but corresponding crystalline material is luminous
Performance is not involved with application.
In this invention, we have studied K2MF7:Mn4+The preparation method of (M is Ta or Nb) luminescent crystal.
Summary of the invention
The object of the present invention is to provide the Mn that one kind can be stimulated by blue light4+The fluoride luminescent crystal of doping.
It is a further object to provide the preparation methods of above-mentioned luminescent crystal.
To achieve the goals above, the Mn according to the present invention being stimulated by blue light4+The fluoride luminescent crystal of doping,
Its chemical composition are as follows: K2M1-xF7:xMn4+；X is corresponding doping Mn4+Ion is with respect to M5+Molar percentage coefficient shared by ion, 0
< x ≤ 0.10；M is Ta or Nb.Raw material type used in the present invention are as follows: potassium fluoride, potassium hexafluoromanganate, tantalum pentoxide or
Niobium pentaoxide, hydrofluoric acid.
Blue light wavelength of the present invention is 420~480 nm.
The above-mentioned Mn being stimulated by blue light4+The preparation method of the fluoride luminescent crystal of doping is using liquid phase crystal growth
Method specifically comprises the following steps: for tantalum pentoxide or niobium pentaoxide to be added in hydrofluoric acid, is vigorously stirred 60 ~ 120 points
Then clock is added potassium hexafluoromanganate and continues stirring 30~60 minutes, potassium fluoride is then added and continues stirring 30~60 minutes.Finally
Acquired solution room temperature is slowly volatilized 7~14 days, orange red strip crystal ethanol washing and in a vacuum drying oven is precipitated
It is 24 hours dry, i.e., required luminescent crystal.
Luminescent crystal of the invention has the very high transparency, and very strong red emission (hair is showed under blue light excitation
Penetrate peak and be located at 628 nm or so), luminous efficiency is high.The emission spectrum CIE value of sample is close to feux rouges NTSC (National
Television Standard Committee) standard value (x = 0.67, y = 0.33)。
Detailed description of the invention
Fig. 1 is K in example 12Ta1-xF7:xMn4+Crystal structure figure；
Fig. 2 is K in example 12Ta1-xF7:xMn4+Photo of the crystal under natural light；
Fig. 3 is K in example 12Ta1-xF7:xMn4+The room temperature excitation spectrum (monitoring wavelength is 628 nm) and emission spectrum of crystal
(excitation wavelength is 468 nm)；
Fig. 4 is K in example 12Ta1-xF7:xMn4+Red-light LED device made by crystal and blue-light LED chip is in 20 mA electric currents
Electroluminescent light spectrogram under excitation；
Fig. 5 is K in example 12Ta1-xF7:xMn4+Crystal and commercial yellow fluorescent powder Y3Al5O12:Ce3+It is made with blue-light LED chip
Electroluminescent light spectrogram of the warm white LED device being made under the excitation of 20 mA electric currents；
Fig. 6 is K in example 22Nb1-xF7:xMn4+Crystal structure figure；
Fig. 7 is K in example 22Nb1-xF7:xMn4+Photo of the crystal under natural light；
Fig. 8 is K in example 22Nb1-xF7:xMn4+The room temperature excitation spectrum (monitoring wavelength is 630 nm) and emission spectrum of crystal
(excitation wavelength is 460 nm).
Specific embodiment
Embodiment 1:
The tantalum pentoxide for weighing 11.05 g, which is added in 25 ml (40 %) hydrofluoric acid (HF), is vigorously stirred 90 minutes, then
The potassium hexafluoromanganate of 0.22 g is added into this solution, and the reaction was continued 30 minutes.The potassium fluoride that 5.81 g then are added continues to stir
60 minutes.Finally gained clear solution room temperature is slowly volatilized 14 days, orange red strip crystal ethanol washing is precipitated 5 times simultaneously
It dries in a vacuum drying oven 24 hours, i.e., required K2TaF7:Mn4+Luminescent crystal.
The structure chart of luminescent crystal thus shown in attached drawing 1, is monoclinic system, and space group isP21/c。
Attached drawing 2 show K2TaF7:Mn4+Photo of the luminescent crystal under natural light, sample show the strip of rule,
With good light transmission.
(excitation wavelength is Fig. 3 for the room temperature excitation spectrum (monitoring wavelength be 628 nm) of luminescent crystal and emission spectrum thus
468 nm).Under the blue light excitation of 468 nm, sample shows a series of red emission peak, wherein most strong emission peak is located at
628 nm.These red emission peaks correspond to Mn4+'s2Eg - 4A2gEnergy level transition.Spectrum CIE coordinate value are as follows:x = 0.687,y= 0.313.Our sample CIE value is close to feux rouges NTSC (National Television Standard
Committee) standard value (x = 0.67, y = 0.33)。
Attached drawing 4 is K2TaF7:Mn4+Luminescent crystal is coated on the white light parts on blue-light semiconductor chip in 20 mA electric currents
Luminescent spectrum under excitation, this device show very strong red emission peak.In figure ~ emission peak of 460 nm is GaN semiconductor
The blue light that chip is issued, we are located at 628 nm in the most strong transmitting of sample.
Attached drawing 5 is K2TaF7:Mn4+Luminescent crystal and business Y3Al5O12:Ce3+The white light being coated on blue-light LED chip
Luminescent spectrum of the LED component under the excitation of 20 mA electric currents.The colour temperature for the white light that this white light parts is issued is 3837 K, colour developing
Index reached 84.
Embodiment 2:
The niobium pentaoxide for weighing 6.65 g, which is added in 25 ml (40 %) hydrofluoric acid (HF), is vigorously stirred 60 minutes, then
The potassium hexafluoromanganate of 0.22 g is added into this solution, and the reaction was continued 30 minutes.The potassium fluoride that 5.81 g then are added continues to stir
60 minutes.Finally gained clear solution room temperature is slowly volatilized 10 days, orange red strip crystal ethanol washing is precipitated 5 times simultaneously
It dries in a vacuum drying oven 24 hours, i.e., required K2NbF7:Mn4+Luminescent crystal.
The structure chart of luminescent crystal thus shown in attached drawing 6, also belongs to monoclinic system, space group isP21/c。
Attached drawing 7 show K2NbF7:Mn4+Photo of the luminescent crystal under natural light, sample show the strip of rule,
With good light transmission.
(excitation wavelength is Fig. 8 for the room temperature excitation spectrum (monitoring wavelength be 630 nm) of luminescent crystal and emission spectrum thus
460 nm).Under the blue light excitation of 460 nm, sample shows a series of red emission peak, wherein most strong emission peak is located at
630 nm.These red emission peaks correspond to Mn4+'s2Eg - 4A2gEnergy level transition.Spectrum CIE coordinate value are as follows:x = 0.688,y= 0.312.Our sample CIE value is close to feux rouges NTSC (National Television Standard
Committee) standard value (x = 0.67, y = 0.33)。
Embodiment 3:
The tantalum pentoxide for weighing 11.05 g, which is added in 25 ml (40 %) hydrofluoric acid (HF), is vigorously stirred 90 minutes, then
The potassium hexafluoromanganate of 0.27 g is added into this solution, and the reaction was continued 60 minutes.The potassium fluoride that 5.81 g then are added continues to stir
60 minutes.Finally gained clear solution room temperature is slowly volatilized 14 days, orange red strip crystal ethanol washing is precipitated 5 times simultaneously
It dries in a vacuum drying oven 24 hours, i.e., required K2TaF7:Mn4+Luminescent crystal.
Embodiment 4:
The tantalum pentoxide for weighing 11.05 g, which is added in 25 ml (40 %) hydrofluoric acid (HF), is vigorously stirred 90 minutes, then
The potassium hexafluoromanganate of 0.27 g is added into this solution, and the reaction was continued 60 minutes.The potassium fluoride that 7.26 g then are added continues to stir
60 minutes.Finally gained clear solution room temperature is slowly volatilized 12 days, orange red strip crystal ethanol washing is precipitated 5 times simultaneously
It dries in a vacuum drying oven 24 hours, i.e., required K2TaF7:Mn4+Luminescent crystal.
Embodiment 5:
The niobium pentaoxide for weighing 6.65 g, which is added in 25 ml (40 %) hydrofluoric acid (HF), is vigorously stirred 60 minutes, then
The potassium hexafluoromanganate of 0.27 g is added into this solution, and the reaction was continued 60 minutes.The potassium fluoride that 5.81 g then are added continues to stir
60 minutes.Finally gained clear solution room temperature is slowly volatilized 12 days, orange red strip crystal ethanol washing is precipitated 5 times simultaneously
It dries in a vacuum drying oven 24 hours, i.e., required K2NbF7:Mn4+Luminescent crystal.
Embodiment 6:
The niobium pentaoxide for weighing 6.65 g, which is added in 25 ml (40 %) hydrofluoric acid (HF), is vigorously stirred 60 minutes, then
The potassium hexafluoromanganate of 0.27 g is added into this solution, and the reaction was continued 60 minutes.The potassium fluoride that 7.26 g then are added continues to stir
60 minutes.Finally gained clear solution room temperature is slowly volatilized 10 days, orange red strip crystal ethanol washing is precipitated 5 times simultaneously
It dries in a vacuum drying oven 24 hours, i.e., required K2NbF7:Mn4+Luminescent crystal.
Claims (4)
1. the Mn that one kind can be stimulated by blue light4+The fluoride luminescent crystal of doping: K2M1-xF7:xMn4+；X is corresponding doping Mn4+From
The opposite M of son5+Molar percentage coefficient shared by ion, 0 < x≤0.10；M is Ta or Nb.
2. the Mn that can be stimulated by blue light as described in claim 14+The fluoride luminescent crystal of doping, it is characterised in that the indigo plant
Light excitation wavelength is the light of 440~480 nm.
3. the Mn that can be stimulated by blue light as described in claim 14+The fluoride luminescent crystal of doping, it is characterised in that preparation side
Method is liquid-phase growth method, includes the following steps: for tantalum pentoxide or niobium pentaoxide to be added in hydrofluoric acid, is vigorously stirred 60
~ 120 minutes, potassium hexafluoromanganate is then added and continues stirring 30~60 minutes, potassium fluoride is then added and continues 30~60 points of stirring
Clock finally slowly volatilizees acquired solution room temperature 7~14 days, and orange red strip crystal ethanol washing is precipitated and does in vacuum
It is 24 hours dry in dry case, i.e., required luminescent crystal.
4. the Mn that can be stimulated by blue light as claimed in claim 34+The preparation method of the fluoride luminescent crystal of doping, feature
The type of raw material used in being are as follows: potassium fluoride, potassium hexafluoromanganate, tantalum pentoxide or niobium pentaoxide, hydrofluoric acid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811201923.8A CN109401752A (en) | 2018-10-16 | 2018-10-16 | A kind of Mn being stimulated by blue light4+The preparation method of the fluoride luminescent crystal of doping |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811201923.8A CN109401752A (en) | 2018-10-16 | 2018-10-16 | A kind of Mn being stimulated by blue light4+The preparation method of the fluoride luminescent crystal of doping |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110423613A (en) * | 2019-07-31 | 2019-11-08 | 中山大学 | A kind of white light LEDs that tetravalence is manganese ion activated large scale emitting red light monocrystal material and preparation method thereof |
| CN116333735A (en) * | 2023-03-28 | 2023-06-27 | 上海应用技术大学 | Tetravalent manganese doped fluoride red fluorescent material with homogeneous core-shell structure and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106554776A (en) * | 2016-10-10 | 2017-04-05 | 云南民族大学 | A kind of effective fluoride red fluorescence powder, preparation method thereof of blue-light semiconductor light-emitting diodes |
| CN107353899A (en) * | 2017-06-15 | 2017-11-17 | 华南理工大学 | A kind of Mn4+Doped fluoride monocrystalline red light material and preparation method and application |
-
2018
- 2018-10-16 CN CN201811201923.8A patent/CN109401752A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106554776A (en) * | 2016-10-10 | 2017-04-05 | 云南民族大学 | A kind of effective fluoride red fluorescence powder, preparation method thereof of blue-light semiconductor light-emitting diodes |
| CN107353899A (en) * | 2017-06-15 | 2017-11-17 | 华南理工大学 | A kind of Mn4+Doped fluoride monocrystalline red light material and preparation method and application |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110423613A (en) * | 2019-07-31 | 2019-11-08 | 中山大学 | A kind of white light LEDs that tetravalence is manganese ion activated large scale emitting red light monocrystal material and preparation method thereof |
| CN116333735A (en) * | 2023-03-28 | 2023-06-27 | 上海应用技术大学 | Tetravalent manganese doped fluoride red fluorescent material with homogeneous core-shell structure and preparation method thereof |
| CN116333735B (en) * | 2023-03-28 | 2024-03-26 | 上海应用技术大学 | Tetravalent manganese doped fluoride red fluorescent material with homogeneous core-shell structure and preparation method thereof |
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