CN108130073A - A kind of tetravalence manganese ion doping indium potassium sodium red fluorescence powder and preparation method - Google Patents
A kind of tetravalence manganese ion doping indium potassium sodium red fluorescence powder and preparation method Download PDFInfo
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- CN108130073A CN108130073A CN201711456152.2A CN201711456152A CN108130073A CN 108130073 A CN108130073 A CN 108130073A CN 201711456152 A CN201711456152 A CN 201711456152A CN 108130073 A CN108130073 A CN 108130073A
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Abstract
The invention discloses a kind of tetravalence manganese ion doping indium potassium sodium red fluorescence powder and preparation method, this crystal structure is cubic system, chemical general formula K2NaInF6:xMn4+, wherein 0.005≤x≤0.07, active ions are tetravalence manganese ion, and after the light source activations such as ultraviolet light or blue light, this fluorescent powder can emit feux rouges, and most strong emission peak is near 631nm.The invention also discloses the preparation methods of such fluorescent powder：It is accurate to weigh indium oxide dissolving in a solution of hydrofluoric acid, quick stirring adds in lithium manganese potassium raw material after 15 minutes, continue stirring 15 minutes, then potassium fluoride and sodium fluoride are added in, stirring stands after 30 minutes and obtains light-yellow precipitate, and indium potassium sodium red fluorescence powder is obtained after centrifuge washing, and equipment and technology requirement is low needed for remarkable advantage of the invention, preparation method is simple, and the fluorescent material of synthesis has good chemical stability.
Description
Technical field
The present invention relates to red fluorescence material fields, more particularly to tetravalence manganese ion doping indium potassium sodium red fluorescence material
Material and preparation method thereof.
Background technology
With the sustainable development of social economy, the problems such as energy shortage, receives more and more attention.It is desirable to
The increasingly consumption of the energy is reduced under the premise of environment is sought protection.In the daily life of the mankind, the electricity of lighting area
Using occupying very big ratio in energy consumption, therefore people need to find novel illumination material instead of traditional lighting.In vain
Light LED has the excellent properties such as small, low energy consumption, luminous efficiency height, service life length, environmental protection as all new generation illumination,
It can replace the illuminating devices such as conventional incandescent, fluorescent lamp.With very wide application prospect.
The main path that current commercialization LED obtains white light includes：(1) multi-chip is combined：Red, green, blue three primary colours chip
It is packaged together, is combined into white light.(2) fluorescent conversion type:The near ultraviolet excitation red, green, blue sent out using UV chip
Three primary colors fluorescent powder utilizes blue chip excitation yellow fluorescent powder (YAG:Ce white light, but blue chip excitation yellow) are obtained
Due to lacking red component, red spectral region shines weaker the LED component that fluorescent powder obtains, and colour developing is usually expressed as in performance and is referred to
Number is low, and colour temperature is more than 4500K, limits the application of its lighting area indoors.Nowadays blue colour fluorescent powder and green emitting phosphor system
Standby technology is ripe, therefore the red fluorescence material for preparing High Efficiency Luminescence is of great significance to improving warm white LED property.
In red fluorescence material, Eu has been had been reported that2+Doped nitride, silicate, aluminate or Ce3+Doping nitridation
The red fluorescence materials such as object, such red fluorescence material have quantum efficiency is high, good chemical stability by
The concern of researcher, however the synthesis technology of such fluorescent powder usually requires high temperature and high pressure environment, reaction condition is required severe
It carves, preparation process is to equipment requirement height, with rare earth ion Eu2+As active ions, emission spectrum is broadband emission, excitation purity
It is low, limit its application in display field.Rare earth ion higher price also improves the manufacturing cost of phosphor material powder simultaneously.
Transient metal Mn4+Outer-shell electron is 3d3Electronic structure, Mn4+Spectral quality there is broadband excitation, narrow emission
Advantage, Mn4+Doped fluoride, oxide, fluorine oxide fluorescent powder can be excited by blue light source, realize red emission.It can be with
It applies in the white light LEDs excited in blue chip.Researcher proposes a series of Mn4+The report of doping fluorescent powder, such as Mn4+
Doped fluoride fluorescent powder (Na2SiF6:Mn4+、K2TiF6:Mn4+、BaTiF6:Mn4+、BaGeF6:Mn4+Deng), Mn4+Doped titanic acid
Salt fluorescent powder (Ga2ZnTiO6:Mn4+、Li2MgTiO4:Mn4+Deng), Mn4+Adulterate germanate fluorescent powder (K2Ge4O9:Mn4+、
SrGe4O9:Mn4+、La3GaGe5O16:Mn4+Deng).Fluoride matrix chemical stability is good, therefore synthesizes in a mild condition occurred frequently
The Mn of light efficiency4+Doped fluoride red fluorescence powder is of great significance.
Invention content
The purpose of the present invention is to provide a kind of indium potassium sodium red fluorescence powder of tetravalence manganese ion doping, such fluorescence
Powder has in ultraviolet light and blue spectrum area to be absorbed, and under ultraviolet light or blue light source excitation, emission spectrum has covering 550-
700nm sections and the centre of luminescence are in 631nm red fluorescences.
Another object of the present invention is to provide above-mentioned novel tetravalence manganese ion doping indium potassium sodium red fluorescence powder
Preparation method, the tetravalence manganese ion present invention uses relative low price as active ions, can at ambient temperature,
The novel tetravalence manganese ion doping indium potassium sodium red fluorescence material with good luminosity is prepared using coprecipitation.
Technical scheme of the present invention：
A kind of tetravalence manganese ion doping indium potassium sodium red fluorescence powder, crystal structure are cubic system, and chemical formula is
K2NaInF6:xMn4+, wherein 0.005≤x≤0.07.
A kind of preparation method of tetravalence manganese ion doping indium potassium sodium red fluorescence powder, includes the following steps:
Step 1：Raw material is weighed, by elemental mole ratios K:Na:In:Mn=40:1:1:X, wherein 0.005≤x≤0.07.
Raw materials of compound of the precise containing potassium respectively, the raw materials of compound containing sodium, the chemical raw material containing manganese, containing indium
Raw materials of compound, fluorine-containing raw materials of compound.
Step 2：The 20mL hydrofluoric acid solutions and 20mL deionized waters that step (1) is weighed are placed in plastic beaker, will be walked
Suddenly after the indium oxide that is weighed in (1) adds in hydrofluoric acid solution, at room temperature with magnetic stirrer 15 minutes, InF is formed6 3-It is molten
Liquid.
Step 3：It is added in weighing in above-mentioned solution containing manganese compound (lithium manganese potassium), continues stirring 15 minutes.
Step 4：Then the sodium fluoride accurately weighed and potassium fluoride raw material are added in, after stirring 30 minutes, beaker is stood 30
Light-yellow precipitate is obtained after minute, is centrifuged, washing for several times, after dry, obtains target product.
The novel tetravalence manganese ion doping indium potassium sodium red fluorescence powder of the present invention has good chemical stability, high
Fluorescence intensity is expected to become a kind of warm white LED red fluorescence material haveing excellent performance.Red fluorescence powder prepared by the present invention
It can be excited by ultraviolet light or blue light, suitable for current blue chip.Under blue light source shooting condition, in 550-
Show the luminosity of red fluorescence in 700nm sections, the centre of luminescence can be applied near~631nm in solid state LED etc.
Display field.The present invention is prepared, this method is simply easy using indium potassium sodium as the red fluorescence material of matrix using coprecipitation
Row, it is low to equipment and technological requirement, high-temperature and high-pressure conditions processing is not needed to, synthesis cycle is short, and preparing at ambient temperature can be with
Obtain the warm white LED red fluorescence material of function admirable.
Description of the drawings
Fig. 1 is K prepared in embodiment 12NaInF6:5%Mn4+The X-ray diffractogram of fluorescent powder；
Fig. 2 is K prepared in embodiment 12NaInF6:5%Mn4+The stereoscan photograph of fluorescent powder；
Fig. 3 is K prepared in embodiment 12NaInF6:5%Mn4+The excitation spectrum and launching light spectrogram of fluorescent powder, should
Figure doubles as
Figure of abstract；
Fig. 4 is K prepared in embodiment 12NaInF6:5%Mn4+The chromatic diagram of fluorescent powder；
Fig. 5 is the launching light spectrogram of fluorescent powder prepared in embodiment 1-5.
Specific embodiment
Embodiment 1:Raw materials of compound containing manganese is lithium manganese potassium, weighs 60mL hydrofluoric acid (40%HF) solution and is placed in modeling
Expect in beaker, add in 0.9g potassium permanganate, at room temperature with magnetic stirrer 10 minutes, form purple solution, weigh 13.4g
Anhydrous potassium fluoride is added in potassium permanganate and hydrofluoric acid mixed solution, continues stirring 15 minutes, 0.7mL 30% is added dropwise
After hydrogenperoxide steam generator, mixed solution gradually becomes yellow from purple, slowly reduces mixing speed, obtains yellow mercury oxide, will produce
Object washs several times, obtains the raw materials of compound containing manganese.It weighs 20mL hydrofluoric acid (40%HF) solution and 20mL deionized waters adds
Enter into plastic beaker, precise 0.3950g indium oxides are dissolved into above-mentioned hydrofluoric acid solution, and magnetic agitation 15 minutes obtains
To InF6 3-Solution.Then the lithium manganese potassium yellow powders of 0.0373g are added in, 0.1260g fluorinations are added in after continuing stirring 15 minutes
Sodium and 6.9719g anhydrous potassium fluorides after being sufficiently stirred 30 minutes, obtain light-yellow precipitate, centrifuge, and washing is for several times, dry
Afterwards, K is obtained2NaInF6:Mn4+Red fluorescence powder.Fig. 1 is synthesized K2NaInF6:Mn4+X-ray diffractogram, X-ray diffraction
Analysis shows the red fluorescence material prepared is consistent with standard card PDF#73-0338, product is pure phase, belongs to cubic system.
K2NaInF6:Mn4+It can be seen that the pattern of sample is irregular polyhedrons (such as Fig. 2) in red fluorescence powder scanned photograph.Fig. 3 is
K2NaInF6:Mn4+The excitation spectrum and launching light spectrogram of red fluorescence powder, shown in figure in 300-550nm regions there are two
Apparent excitation peak matches in~470nm excitation peaks and blue chip commercial at present, can when 470nm is as excitation wavelength
To generate red emission peak, peak position is located near 631nm.K2NaInF6:Mn4+The chromatic diagram (Fig. 4) of fluorescent powder shows prepared
The chromaticity coordinates of product is located at red light region (x=0.6721, y=0.3277).Fig. 5 is red fluorescence material K2NaInF6:Mn4+
The launching light spectrogram of (0.005≤x≤0.07), as can be seen from FIG. 5 novel tetravalence manganese ion doping indium potassium sodium red fluorescence
For powder doping concentration in x=0.05 or so, luminous intensity is best.
Embodiment 2:Chemical raw material containing manganese is lithium manganese potassium, and preparation process is similar with embodiment 1.Weigh 20mL
Hydrofluoric acid (40%HF) solution and 20mL deionized waters are added in plastic beaker, and precise 0.4139g indium oxides are dissolved into
In above-mentioned hydrofluoric acid solution, magnetic agitation 15 minutes obtains InF6 3-Solution.Then the lithium manganese potassium yellow powder of 0.0036g is added in
End adds in 0.1259g sodium fluorides and 6.9715g anhydrous potassium fluorides after continuing stirring 15 minutes, after being sufficiently stirred 30 minutes, obtains
Light-yellow precipitate centrifuges, and washing for several times, after dry, obtains K2NaInF6:Mn4+Red fluorescence powder.X-ray diffraction analysis
Show the pure phase that the red fluorescence material prepared is indium potassium sodium.The spectral quality of fluorescent powder is similar with embodiment 1.
Embodiment 3:Chemical raw material containing manganese is lithium manganese potassium, and preparation process is similar with embodiment 1.Weigh 20mL
Hydrofluoric acid (40%HF) solution and 20mL deionized waters are added in plastic beaker, and precise 0.4116g indium oxides are dissolved into
In above-mentioned hydrofluoric acid solution, magnetic agitation 15 minutes obtains InF6 3-Solution.Then the lithium manganese potassium yellow powder of 0.0077g is added in
End adds in 0.1256g sodium fluorides and 6.9727g anhydrous potassium fluorides after continuing stirring 15 minutes, after being sufficiently stirred 30 minutes, obtains
Light-yellow precipitate centrifuges, and washing for several times, after dry, obtains K2NaInF6:Mn4+Red fluorescence powder.X-ray diffraction analysis
Show the pure phase that the red fluorescence material prepared is indium potassium sodium.The spectral quality of fluorescent powder is similar with embodiment 1.
Embodiment 4:Chemical raw material containing manganese is lithium manganese potassium, and preparation process is similar with embodiment 1.Weigh 20mL
Hydrofluoric acid (40%HF) solution and 20mL deionized waters are added in plastic beaker, and precise 0.4030g indium oxides are dissolved into
In above-mentioned hydrofluoric acid solution, magnetic agitation 15 minutes obtains InF6 3-Solution.Then the lithium manganese potassium yellow powder of 0.0224g is added in
End adds in 0.1255g sodium fluorides and 6.9724g anhydrous potassium fluorides after continuing stirring 15 minutes, after being sufficiently stirred 30 minutes, obtains
Light-yellow precipitate centrifuges, and washing for several times, after dry, obtains K2NaInF6:Mn4+Red fluorescence powder.X-ray diffraction analysis
Show the pure phase that the red fluorescence material prepared is indium potassium sodium.The spectral quality of fluorescent powder is similar with embodiment 1.
Embodiment 5:Chemical raw material containing manganese is lithium manganese potassium, and preparation process is similar with embodiment 1.Weigh 20mL
Hydrofluoric acid (40%HF) solution and 20mL deionized waters are added in plastic beaker, and precise 0.3877g indium oxides are dissolved into
In above-mentioned hydrofluoric acid solution, magnetic agitation 15 minutes obtains InF6 3-Solution.Then the lithium manganese potassium yellow powder of 0.0522g is added in
End adds in 0.1257g sodium fluorides and 6.9720g anhydrous potassium fluorides after continuing stirring 15 minutes, after being sufficiently stirred 30 minutes, obtains
Light-yellow precipitate centrifuges, and washing for several times, after dry, obtains K2NaInF6:Mn4+Red fluorescence powder.X-ray diffraction analysis
Show the pure phase that the red fluorescence material prepared is indium potassium sodium.The spectral quality of fluorescent powder is similar with embodiment 1.
Embodiment 6:Chemical raw material containing manganese is lithium manganese potassium, and preparation process is similar with embodiment 1.Weigh 20mL
Hydrofluoric acid (40%HF) solution and 20mL deionized waters are added in plastic beaker, and precise 0.3953g indium oxides are dissolved into
In above-mentioned hydrofluoric acid solution, magnetic agitation 15 minutes obtains InF6 3-Solution.Then the lithium manganese potassium yellow powder of 0.0377g is added in
End adds in 0.4082g sodium acetates and 6.9719g anhydrous potassium fluorides after continuing stirring 15 minutes, after being sufficiently stirred 30 minutes, obtains
Light-yellow precipitate centrifuges, and washing for several times, after dry, obtains K2NaInF6:Mn4+Red fluorescence powder.X-ray diffraction analysis
Show the pure phase that the red fluorescence material prepared is indium potassium sodium.The spectral quality of fluorescent powder is similar with embodiment 1.
Embodiment 7:Chemical raw material containing manganese is lithium manganese potassium, and preparation process is similar with embodiment 1.Weigh 20mL
Hydrofluoric acid (40%HF) solution and 20mL deionized waters are added in plastic beaker, and precise 0.3952g indium oxides are dissolved into
In above-mentioned hydrofluoric acid solution, magnetic agitation 15 minutes obtains InF6 3-Solution.Then the lithium manganese potassium yellow powder of 0.0373g is added in
End adds in 0.1755g sodium chloride and 6.9711g anhydrous potassium fluorides after continuing stirring 15 minutes, after being sufficiently stirred 30 minutes, obtains
Light-yellow precipitate centrifuges, and washing for several times, after dry, obtains K2NaInF6:Mn4+Red fluorescence powder.X-ray diffraction analysis
Show the pure phase that the red fluorescence material prepared is indium potassium sodium.The spectral quality of fluorescent powder is similar with embodiment 1.
Claims (4)
1. a kind of red fluorescence powder of tetravalence manganese ion doping indium potassium sodium, which is characterized in that be prepared for using coprecipitation
Tetravalence manganese ion doping indium potassium sodium red fluorescence powder, the fluorescent powder belong to cubic phase, molecular formula K2NaInF6:Mn4+,
Active ions are Mn4+Ion.
2. red fluorescence powder according to claim 1, which is characterized in that the launch wavelength of the red fluorescence powder is located at
550-700nm, emission peak are located near 631nm.
3. a kind of preparation method of tetravalence manganese ion doping indium potassium sodium red fluorescence powder, which is characterized in that including walking as follows
Suddenly：
Step 1：Raw material is weighed, by elemental mole ratios K:Na:In:Mn=40:1:1:X, wherein 0.005≤x≤0.07, accurate respectively
Really raw materials of compound of the weighing containing potassium, the raw materials of compound containing sodium, the chemical raw material containing manganese, the raw materials of compound containing indium contain
The raw materials of compound of fluorine；
Step 2：The 20mL hydrofluoric acid solutions and 20mL deionized waters that step (1) is weighed are placed in plastic beaker, by step (1)
In after the indium oxide that weighs adds in hydrofluoric acid solution, at room temperature with magnetic stirrer 15 minutes, form InF6 3-Solution；
Step 3：It is added in weighing in above-mentioned solution containing manganese compound (lithium manganese potassium), continues stirring 15 minutes；
Step 4：Then the sodium fluoride accurately weighed and potassium fluoride raw material are added in, is stirred 30 minutes, after beaker is stood 30 minutes
Light-yellow precipitate is obtained, is centrifuged, washing for several times, after dry, obtains target product.
4. preparation method according to claim 3, which is characterized in that the raw materials of compound containing sodium be sodium fluoride, chlorine
Change sodium, any one in sodium acetate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109294566A (en) * | 2018-10-29 | 2019-02-01 | 温州大学 | A kind of fluorine indium acid barium red fluorescence powder and preparation method thereof that tetravalence is manganese ion activated |
| CN112358870A (en) * | 2020-10-28 | 2021-02-12 | 深圳大学 | Lead-free indium-based double perovskite material and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2733494A1 (en) * | 1995-04-28 | 1996-10-31 | Centre Nat Rech Scient | New caesium magnesium indium fluoride crystal used as scintillator or neutrino detector |
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2017
- 2017-12-28 CN CN201711456152.2A patent/CN108130073A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2733494A1 (en) * | 1995-04-28 | 1996-10-31 | Centre Nat Rech Scient | New caesium magnesium indium fluoride crystal used as scintillator or neutrino detector |
Non-Patent Citations (2)
| Title |
|---|
| L.Y.WANG等: "Luminescence properties and warm white LED application of a ternary-alkaline fluoride red phosphor K2NaAlF6:Mn4+", 《DALTON TRANSACTIONS》 * |
| SHIJIE QIU等: "Synthesis and photoluminescence of Mn4+ activated ternary-alkaline fluoride K2NaGaF6 red phosphor for warm-white LED application", 《RSC ADVANCES》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109294566A (en) * | 2018-10-29 | 2019-02-01 | 温州大学 | A kind of fluorine indium acid barium red fluorescence powder and preparation method thereof that tetravalence is manganese ion activated |
| CN112358870A (en) * | 2020-10-28 | 2021-02-12 | 深圳大学 | Lead-free indium-based double perovskite material and preparation method and application thereof |
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