CN106800930A - A kind of oxyfluoride red fluorescence powder of Mn (IV) activation and preparation method thereof - Google Patents
A kind of oxyfluoride red fluorescence powder of Mn (IV) activation and preparation method thereof Download PDFInfo
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Abstract
Oxyfluoride red fluorescence powder the invention discloses a kind of Mn (IV) activation and preparation method thereof, fluorescent material formula A2‑xBx(MoO2F4)H2O:Mn4+ yThe material composition of expression, A, B each independent representative Na, K, Cs or Rb in formula, and A, B differ, the value of x are 0.03~0.16 for the value of 0~1, y, and it is by K2MnF6And MoO3、A2‑xHF2、BxHF2Mixture 100~180 DEG C of insulations are prepared from for 12~24 hours in confined conditions.Preparation process raw material of the present invention is easily well mixed, without hydrofluoric acid, it is pollution-free, technical process is simple, activation agent content is controllable, and prepared light-emitting phosphor intensity is high, powder granularity is controllable, luminescent properties are good, is adapted to the field higher to luminescent material requirement such as White-light LED illumination device and backlight.
Description
Technical field
The invention belongs to luminescent material technical field, and in particular to a kind of oxyfluoride red fluorescence powder of Mn (IV) activation
And preparation method thereof.
Background technology
At present, luminescent material has become the backing material in the fields such as presentation of information, lighting source, photoelectric device, fluorescence
The high luminous intensity of powder and good micro-shape can effectively improve the performance of display, therefore, novel fluorescent material
Research and application always one of important research field of materials chemistry and materials physics.
White light-emitting diode (WLEDs) since the invention in 1996, its energy-conservation and it is environment-friendly the characteristics of make people couple
It has been sent in unlimited hope, and every property of the luminescent material for WLEDs, such as chromaticity coordinates, associated temperature coefficient etc. have
Very important effect.YAG:Ce3+Generation white light is combined with the blue chip of LED earliest and turns into widely used in WLEDs
Due to lacking emitting red light composition in business yellow fluorescent powder, but the WLEDs for so combining, there is low excitation, Gao Xiang
The shortcomings of closing temperature coefficient, it is difficult to be applied to the backlight of general lighting and display device.
Although researcher targetedly develops such as red fluorescence powder such as nitride, fluoride, preparation condition
Harshness makes its manufacturing cost remain high, and the broadband emission of nitride red fluorescent powder and low excitation are seriously constrained
Its application in display device backlight source.Composition, heat treatment time and the temperature for being fluorinated matter fluorescent powder are to determine fluorescent material hair
The key factor of optical property.By controlling composition, heat treatment temperature, the time of fluorescent material, can prepare that luminous intensity is high, powder
The smooth fluorination matter fluorescent powder of regular particles, particle surface.In recent years, a series of fluoride red fluorescence powder of Mn (IV) activation
(formula is Aa-xBxMX6:Mn4+ yThe material composition of expression, M represents Si, Ge, Ti, Sn or Zr in formula, and X represents halogen, and y represents Mn4 +Molal quantity, the value of y is 0.03~0.16, a=1 or 2, and during wherein a=1, the value of x is 0~1, and A, B are each independent
Na, K, Cs or Rb are represented, during a=2, the value of x is 0~2, A, B each independent representative Mg, Ba or Zn, and A, B are differed)
Red fluorescence powder is attracted attention.Such as Mn4+The K of activation2TiF6Excitation spectrum can ultraviolet with LED well and indigo plant
Color chip is luminous to match, and in 500K without obvious light decay.
The formula of the fluoride red fluorescence powder of existing Mn (IV) activation is Aa-xBxMX6:Mn4+ y, synthesizing, this type of red is glimmering
It is bar none all to use HF as solvent during light powder.Largely there is potential safety hazard using HF.Furthermore in fluorescent material
Preparation process in, the ratio of activator is uncertain, quite a few activator ion Mn in synthesized fluorescent material4+In the presence of
In the middle of liquid phase, activator wastage of material will certainly be caused.And the concentration of the activator ion in product relies on subsequent analysis
Just can determine that.Therefore a kind of synthetic system without HF is developed, and can accurately controls to activate agent content and Mn simple to operate (IV)
The red fluorescence powder of activation becomes industry and is badly in need of.
The content of the invention
The technical problems to be solved by the invention are that a kind of luminous intensity of offer is high, granularity is controllable, long service life
The oxyfluoride red fluorescence powder of Mn (IV) activation, and for the red fluorescence powder provides it is a kind of it is simple to operate, without HF pollutions, activate
The controllable preparation method of agent ion.
Solving the technical scheme that is used of above-mentioned technical problem is:Fluorescent material formula A2-xBx(MoO2F4)H2O:Mn4+ y
The material composition of expression, A, B each independent representative Na, K, Cs or Rb in formula, and A, B are differed, and the value of x is 0~1, y's
Value is 0.03~0.16.
The formula A of above-mentioned fluorescent material2-xBx(MoO2F4)H2O:Mn4+ yIn, preferably the value of x represents Na or K for 0, A.
The formula A of above-mentioned fluorescent material2-xBx(MoO2F4)H2O:Mn4+ yIn, the value of further preferred y is 0.06~0.12.
The preparation method of the oxyfluoride red fluorescence powder of Mn (IV) of the present invention activation is:According to K2(MoO2F4)H2O:Mn4 + 0.10Stoichiometric proportion weigh raw material K2MnF6、MoO3、A2-xHF2、BxHF2, ground in mortar after raw material is well mixed, so
Afterwards in confined conditions 100~180 DEG C be incubated 12~24 hours, be cooled to normal temperature, product uses acetone, deionized water, nothing successively
After water-ethanol washing, vacuum drying obtains the oxyfluoride red fluorescence powder of Mn (IV) activation.
In the preparation method of the oxyfluoride red fluorescence powder of above-mentioned Mn (IV) activation, preferably in confined conditions 150 DEG C
Insulation 12 hours.
The present invention synthesizes Mn using the oxyfluoride red fluorescence powder of Solid phase synthesis Mn (IV) activation compared to other
(IV) method of the fluoride red fluorescence powder of activation has the following advantages that:
1st, the present invention is simple to operate, and synthesis step only has a step, and reaction time is short, and course of reaction is easily controllable, has greatly
Business potential.
2nd, environmental protection of the present invention, compared with precipitation method synthesis fluoride red fluorescence powder needs substantial amounts of hydrofluoric acid, instead
Should in do not need hydrofluoric acid, solve serious pollution problem in product building-up process, greatly reduce potential safety hazard.
3rd, the ratio of activator is controllable in the red fluorescence powder of present invention synthesis, does not result in activator wastage of material, saves
About medicine, low cost.
4th, light-emitting phosphor intensity of the present invention is high, granularity is controllable, stability is high, long service life, entirely appropriate white light LEDs
The requirement of device, with important industrial application value.
Brief description of the drawings
Fig. 1 is K prepared by embodiment 1~32(MoO2F4)H2O:Mn4+ 0.10The X-ray diffractogram of red fluorescence powder.
Fig. 2 is K prepared by embodiment 1~32(MoO2F4)H2O:Mn4+ 0.10The launching light spectrogram of red fluorescence powder.
Fig. 3 is K prepared by embodiment 12(MoO2F4)H2O:Mn4+ 0.10The stereoscan photograph of red fluorescence powder.
Fig. 4 is Na prepared by embodiment 42(MoO2F4)H2O:Mn4+ 0.08The X-ray diffractogram of red fluorescence powder.
Fig. 5 is red fluorescence powder Na prepared by embodiment 4~62(MoO2F4)H2O:Mn4+ 0.08、Na2(MoO2F4)H2O:Mn4 + 0.10、Na2(MoO2F4)H2O:Mn4+ 0.12Launching light spectrogram.
Fig. 6 is Na prepared by embodiment 42(MoO2F4)H2O:Mn4+ 0.08The stereoscan photograph of red fluorescence powder.
Fig. 7 is Rb prepared by embodiment 72(MoO2F4)H2O:Mn4+ 0.12The X-ray diffractogram of red fluorescence powder.
Fig. 8 is Rb prepared by embodiment 72(MoO2F4)H2O:Mn4+ 0.12The launching light spectrogram of red fluorescence powder.
Fig. 9 is Rb prepared by embodiment 72(MoO2F4)H2O:Mn4+ 0.12The stereoscan photograph of red fluorescence powder.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.
K used in example below2MnF6Preparation method be:By 6.4g KMnO4With 128.0g KHF2It is placed in
In 1000mL plastic measuring glass, in adding 420mL mass fractions to be 49% aqueous hydrogen fluoride solution, ice bath stirring in confined conditions
It is completely dissolved to solid, is then added dropwise over the H that 5.10mL mass fractions are 30%2O2The aqueous solution, drips rear stirring at normal temperature 30
Minute, stratification outwells supernatant liquor, and precipitation is respectively washed 3 times with the hydrofluoric acid and acetone of mass fraction 20%, 60 DEG C of dryings
4 hours, obtain K2MnF6。
Embodiment 1
According to K2(MoO2F4)H2O:Mn4+ 0.10Stoichiometric proportion, by 0.175g MoO3With 0.070g K2MnF6Mixing,
Add 0.187g KHF2, after being fully ground in mortar, it is transferred in the reactor of polytetrafluoroethyllining lining, at 150 DEG C
Sealing thermal insulation 24 hours, is cooled to normal temperature after having reacted, precipitation is respectively washed 3 times with acetone, deionized water, absolute ethyl alcohol successively,
110 DEG C are vacuum dried 4 hours, obtain K2(MoO2F4)H2O:Mn4+ 0.10Red fluorescence powder.
Embodiment 2
In the present embodiment, sealing thermal insulation 24 hours at 130 DEG C, other steps are same as Example 1, obtain K2
(MoO2F4)H2O:Mn4+ 0.10Red fluorescence powder.
Embodiment 3
In the present embodiment, sealing thermal insulation 24 hours at 170 DEG C, other steps are same as Example 1, obtain K2
(MoO2F4)H2O:Mn4+ 0.10Red fluorescence powder.
The Rigaku mini flex 6000 that fluorescent material prepared by embodiment 1~3 is produced using Rigaku Co., Ltd.
Type x-ray powder diffraction instrument carries out material phase analysis to product, and (test condition is:CuK α are radiated, and voltage is 40KV, and electric current is
15mA, sweep limits is 10 °~50 °, and sweep speed is 10 °/min, and step-length is 0.02 °), the F- produced using Hitachi, Ltd
The test of 4600 XRFs carries out luminescent properties measurement, the desk-top scanning electron of TM3030 types produced using HIT
Microscope (SEM) observes the pattern of product grain, while the type environmental scannings of Quanta 200 electricity produced using FEI Co. of the U.S.
Sub- microscope (SEM) observes the pattern of particle, as a result sees Fig. 1~3.
As seen from Figure 1, the diffraction maximum and K of the fluorescent material prepared by embodiment 1~32(MoO2F4)H2O standard cards are consistent,
And thing compare it is pure, without obvious dephasign exist.Seen by Fig. 2, the fluorescent material prepared by embodiment 1~3 is sent out under 460nm exciting lights
Peak value is penetrated at 630nm, belongs to Mn4+'s2Eg→4A2gCharacteristic transition is launched, and illustrates that sample glows, wherein swashing in 460nm
Under luminous, launch wavelength at 630nm, the relative luminous intensity of the red fluorescence powder of embodiment 1 is the red of 8935, embodiment 2
The relative luminous intensity of color fluorescent material is that the relative luminous intensity of the red fluorescence powder of 6515, embodiment 3 is 5949.Complex chart 1
It is K with 2 explanation gained fluorescent material2(MoO2F4)H2O:Mn4+ 0.10Red fluorescence powder, and luminous intensity is high, excitation preferably, can be used
In white light LEDs.As seen from Figure 3, the fluorescent powder grain that prepared by embodiment 1 is evenly distributed, particle size uniformity, at 30 μm or so.
Embodiment 4
According to Na2(MoO2F4)H2O:Mn4+ 0.08Stoichiometric proportion, by 0.175g MoO3With 0.056g K2MnF6Mixing,
Add 0.149g NaHF2, other steps are same as Example 1, obtain Na2(MoO2F4)H2O:Mn4+ 0.08Red fluorescence powder.
Embodiment 5
According to Na2(MoO2F4)H2O:Mn4+ 0.10Stoichiometric proportion, by 0.175g MoO3With 0.07g K2MnF6Mixing,
Add 0.149g NaHF2, other steps are same as Example 1, obtain Na2(MoO2F4)H2O:Mn4+ 0.10Red fluorescence powder.
Embodiment 6
According to Na2(MoO2F4)H2O:Mn4+ 0.12Stoichiometric proportion, by 0.175g MoO3With 0.07g K2MnF6Mixing,
Add 0.149g NaHF2, other steps are same as Example 1, obtain Na2(MoO2F4)H2O:Mn4+ 0.12Red fluorescence powder.
From fig. 4, it can be seen that the diffraction maximum and Na of fluorescent material prepared by embodiment 42(MoO2F4)H2O:Mn4+ 0.08Standard card
Unanimously, and thing compare it is pure, without obvious dephasign exist.As seen from Figure 5, the fluorescent material prepared by embodiment 4~6 is excited in 460nm
Under light, emission peak belongs to Mn at 630nm4+'s2Eg→4A2gCharacteristic transition is launched, and illustrates that sample glows, wherein
Under 460nm exciting lights, launch wavelength at 630nm, the relative luminous intensity of the red fluorescence powder of embodiment 4 is 7612, implements
The relative luminous intensity of the red fluorescence powder of example 5 is that the relative luminous intensity of the red fluorescence powder of 5452, embodiment 6 is 5017.
Comprehensive Figure 4 and 5 explanation gained red light emitting phosphor intensity is high, and excitation preferably, can be used for white light LEDs.As seen from Figure 6, it is real
Apply the fluorescent powder grain prepared by example 4 to be evenly distributed, particle size uniformity, at 30 μm or so.
Embodiment 7
According to Rb2(MoO2F4)H2O:Mn4+ 0.12Stoichiometric proportion, by 0.175g MoO3With 0.07g K2MnF6Mixing,
Add 0.300g RbHF2, other steps are same as Example 1, obtain Rb2(MoO2F4)H2O:Mn4+ 0.12Red fluorescence powder.
As seen from Figure 7, the diffraction maximum and Rb of prepared fluorescent material2(MoO2F4)H2O:Mn4+ 0.12Standard card is consistent, and
Thing compare it is pure, without obvious dephasign exist.As seen from Figure 8, under 460nm exciting lights, emission peak is located at prepared fluorescent material
At 630nm, belong to Mn4+'s2Eg→4A2gCharacteristic transition is launched, and illustrates that sample glows, and it is under 460nm exciting lights, transmitted wave
Relative luminous intensity at 630nm long is 5184, illustrates that sample luminous intensity is high, and excitation preferably, can be used for white light LEDs.
As seen from Figure 9, prepared fluorescent powder grain is evenly distributed, particle size uniformity, at 20 μm or so.
Embodiment 8
According to Na0.2K1.8(MoO2F4)H2O:Mn4+ 0.12Stoichiometric proportion, by 0.175g MoO3With 0.07g K2MnF6It is mixed
Close uniform, add 0.0148g NaHF2、0.169g KHF2, other steps are same as Example 1, obtain Na0.2K1.8
(MoO2F4)H2O:Mn4+ 0.12Red fluorescence powder.
Embodiment 9
According to Na0.4K1.6(MoO2F4)H2O:Mn4+ 0.12Stoichiometric proportion, by 0.175g MoO3With 0.07g K2MnF6It is mixed
Close uniform, add 0.0296g NaHF2、0.150g KHF2, other steps are same as Example 1, obtain Na0.4K1.6
(MoO2F4)H2O:Mn4+ 0.12Red fluorescence powder.
Embodiment 10
According to NaK (MoO2F4)H2O:Mn4+ 0.12Stoichiometric proportion, by 0.175g MoO3With 0.07g K2MnF6Mixing is equal
It is even, add 0.074g NaHF2、0.094g KHF2, other steps are same as Example 1, obtain NaK (MoO2F4)H2O:Mn4 + 0.12Red fluorescence powder.
Embodiment 11
According to Na1.4K0.6(MoO2F4)H2O:Mn4+ 0.12Stoichiometric proportion, by 0.175g MoO3With 0.07g K2MnF6It is mixed
Close uniform, add 0.104g NaHF2、0.056g KHF2, other steps are same as Example 1, obtain Na1.4K0.6
(MoO2F4)H2O:Mn4+ 0.12Red fluorescence powder.
Embodiment 12
According to Na1.8K0.2(MoO2F4)H2O:Mn4+ 0.12Stoichiometric proportion, by 0.175g MoO3With 0.07g K2MnF6It is mixed
Close uniform, add 0.134g NaHF2、0.019g KHF2, other steps are same as Example 1, obtain Na1.8K0.2
(MoO2F4)H2O:Mn4+ 0.12Red fluorescence powder.
Under 460nm exciting lights, emission peak belongs to fluorescent material prepared by above-described embodiment 8~12 at 630nm
Mn4+'s2Eg→4A2gCharacteristic transition is launched, and illustrates that sample glows, and luminous intensity is high, and excitation preferably, can be used for white light
LED.Fluorescent powder grain is evenly distributed, particle size uniformity, at 20 μm or so.The diffraction maximum of fluorescent material is by K2(MoO2F4)H2O:
Mn4+ 0.10Gradually become Na2(MoO2F4)H2O:Mn4+ 0.10Standard card is consistent, and thing is compared pure, is existed without obvious dephasign.
Claims (5)
1. the oxyfluoride red fluorescence powder that a kind of Mn (IV) is activated, it is characterised in that:Fluorescent material formula A2-xBx
(MoO2F4)H2O:Mn4+ yThe material composition of expression, A, B each independent representative Na, K, Cs or Rb in formula, and A, B are differed, x
Value for 0~1, y value be 0.03~0.16.
2. the oxyfluoride red fluorescence powder that Mn (IV) according to claim 1 is activated, it is characterised in that:The x's takes
Be worth is that 0, A represents Na or K.
3. the oxyfluoride red fluorescence powder that Mn (IV) according to claim 1 and 2 is activated, it is characterised in that:The y's
Value is 0.06~0.12.
4. a kind of preparation method of the oxyfluoride red fluorescence powder of Mn (IV) activation described in claim 1, it is characterised in that:
According to K2(MoO2F4)H2O:Mn4+ 0.10Stoichiometric proportion weigh raw material K2MnF6、MoO3、A2-xHF2、BxHF2, raw material is mixed
Ground in mortar after uniform, then in confined conditions 100~180 DEG C be incubated 12~24 hours, be cooled to normal temperature, product according to
After secondary use acetone, deionized water, absolute ethanol washing, vacuum drying obtains the oxyfluoride red fluorescence powder of Mn (IV) activation.
5. the preparation method of the oxyfluoride red fluorescence powder of Mn (IV) according to claim 4 activation, it is characterised in that:
150 DEG C are incubated 12 hours in confined conditions.
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WO2019179907A1 (en) | 2018-03-20 | 2019-09-26 | Merck Patent Gmbh | Mn-activated oxidohalides as conversion luminescent materials for led-based solid state light sources |
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JP7326313B2 (en) | 2018-03-20 | 2023-08-15 | リテック-フェアメーゲンスフェアヴァルトゥングスゲゼルシャフト ミット ベシュレンクテル ハフツング | Mn-activated oxide halides as conversion luminescent materials for LED-based solid-state light sources |
TWI814793B (en) * | 2018-03-20 | 2023-09-11 | 德商利特資產管理公司 | Mn-activated oxidohalides as conversion luminophores for led-based solid-state light sources |
CN110511755A (en) * | 2019-09-10 | 2019-11-29 | 云南民族大学 | A kind of indigo plant is light activated to mix the molybdate red luminescent material of Mn4+ |
WO2022110747A1 (en) * | 2020-11-30 | 2022-06-02 | 华南理工大学 | Molybdate luminescent ceramic material for laser display, preparation method therefor and use thereof |
CN112410030A (en) * | 2020-12-03 | 2021-02-26 | 重庆文理学院 | Preparation method of multiphase composite molybdate oxyfluoride nano fluorescent material |
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