CN109111923A - One kind can be by ultraviolet light, black light or blue light activated red fluorescence powder and preparation method thereof - Google Patents
One kind can be by ultraviolet light, black light or blue light activated red fluorescence powder and preparation method thereof Download PDFInfo
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- CN109111923A CN109111923A CN201811171041.1A CN201811171041A CN109111923A CN 109111923 A CN109111923 A CN 109111923A CN 201811171041 A CN201811171041 A CN 201811171041A CN 109111923 A CN109111923 A CN 109111923A
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
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Abstract
The invention discloses one kind can be by ultraviolet light, black light or blue light activated red fluorescence powder and preparation method thereof, the chemical formula of red fluorescence powder are as follows: NaLa0.7(MoO4)2‑x(WO4)x:0.3Eu3+, wherein x=0,0.5,1,1.5 or 2；Preparation method includes the following steps: s1. weighs a certain amount of La2O3、MoO3、Eu2O3、WO3、Na2CO3Raw material；S2. weighed each raw material is mixed and is put into ball grinder, and suitable dehydrated alcohol is added according to the fluorescent powder total amount of required preparation；S3. the ball grinder equipped with sample is placed in ball mill after ball milling with washes of absolute alcohol ball grinder and agate ball；S4. sample is put into thermostatic drying chamber and is dried, and the resulting powder of drying is fully ground, then be pressed into block with tablet press machine；S5. the block is placed in alumina crucible, is put into box high temperature sintering furnace and is sintered, that is, obtain the fluorescent powder.Red fluorescence powder of the invention can effectively be excited by black light 393nm and blue light 462nm, and transmitting main peak is located at 615nm, and luminous intensity is with W6+The increase of doping concentration and increase, work as W6+It shines when doping x=1 most strong, and feux rouges excitation purity is best.
Description
Technical field
The invention belongs to fluorescent powder and its preparation fields, and in particular to one kind can be swashed by ultraviolet light, black light or blue light
Red fluorescence powder of hair and preparation method thereof.
Background technique
White light emitting diode is as 21 century a new generation's energy-conserving light source.Realize the important channel of white light first is that benefit
With the body fluorescence conversion technology of rare earth luminescent material, the 460nm blue light or 400nm black light that InGaN semiconductor element is emitted
It is converted into white light.Realize that there are mainly three types of methods for white light at present, but there is no full maturitys, thus severely impact white light LEDs
In the application of lighting area.Specifically, first method is that the yellow that can be stimulated by blue light is applied on blue LED die
Fluorescent powder, the yellow light that the blue light and fluorescent powder that chip issues issue are complementarily shaped to white light.Day sub- chemistry, Ou Silang etc. are obtained respectively
Obtained and be made the patents of white light LEDs using such fluorescent powder matching blue-ray LED, but day Asia patent US5998925 provide it is logical
Formula is (Y1-x,Gdx)3(Al1–y,Gay)5O12: Ce (referred to as YAG: Ce), and the chemistry that Ou Silang patent US6669866 is provided
Formula is TAG:Ce, but since the TAG:Ce application for being still difficult to catch up with and surpass YAG: Ce, TAG:Ce in terms of luminous efficiency is also difficult to
It is promoted.One disadvantage of this scheme is exactly Ce in the fluorophor3+The emission spectrum of ion does not have continuous spectrum characteristic,
Colour rendering is poor, it is difficult to meet the requirement of low color temperature illumination, while luminous efficacy is high not enough, need novel by developing
High-efficiency fluorescence powder improves；Second of implementation method is that green and red fluorescence powder are coated on blue LED die, passes through chip
Green light that the blue light of sending and fluorescent powder issue and feux rouges is compound obtains white light, colour rendering is preferable, however all the time, LED
Alkaline earth sulfide series is confined to red fluorescence powder, such fluorescent powder physicochemical properties is extremely unstable, and heat is steady more
Qualitative difference, light decay is big, seriously compromises the quality of white light LEDs product, and many LED are developed successively with new red phosphors
Out, such as silicate, tungsten hydrochlorate, aluminate and nitrogen (oxygen) compound fluorophor；The third implementation method be in purple light or
The fluorescent powder that three primary colours or multiple color are applied on ultraviolet leds chip, utilizes the long wave ultraviolet light (370nm of the chip emission
~380nm) or purple light (380nm~410nm) carry out excitated fluorescent powder and realize white light emission, this method colour rendering is more preferable, but same
Sample there is a problem of similar with second method.Therefore it develops efficient low light attenuation and cheap phosphor for white light LED has become
For an extremely urgent job and current the main direction of development.
Yang Zhi equal utilization high temperature solid-state method has synthesized SrMoO within 20064:Eu3+Red fluorescence powder, its excitation spectrum are
Two peak structure, two main peaks are located at the near ultraviolet band of 394nm and the blue visible light area of 464nm, and emission spectra is line spectrum, main
Peak-to-peak value is 624nm, this is the good feux rouges that can meet with ultraviolet and blue chip.Han Yong etc. is ground in absorption Yang Zhi equality
Study carefully on the basis of achievement in SrMoO4:Eu3+Middle addition Na+, and using it as compensation charge, due to parent lattice, swash
The broadband of luminous spectrum extends to 350nm, can preferably absorb the spectrum that blue led is issued, and light emission luminance improves 25% left side
It is right.
Summary of the invention
The purpose of the present invention is: develop a kind of red that the property that can be effectively excited by black light or blue light is stable
Fluorescent powder and preparation method thereof.
To realize the above-mentioned technical purpose, The technical solution adopted by the invention is as follows:
One kind can be by ultraviolet light, black light or blue light activated red fluorescence powder, chemical formula are as follows: NaLa0.7
(MoO4)2-x(WO4)x:0.3Eu3+, wherein x=0,0.5,1,1.5 or 2.
Further, the fluorescent powder can be excited by the blue light of the black light of 393nm and 462nm, emission spectrum by
Multiple groups spike composition between 585-630nm, wherein the luminous intensity at 615nm is maximum；
Further, the fluorescent powder can improve luminous intensity by introducing wolframic acid, and work as W6+Replace Mo6+Doping ratio
When example is 1, the luminous intensity of sample is maximum；
Further, red twilight sunset can be obtained after being stopped with 254nm ultraviolet excitation in the fluorescent powder.
The invention also discloses the preparation methods of above-mentioned red fluorescence powder, comprising the following steps:
S1. a certain amount of La is weighed2O3、MoO3、Eu2O3、WO3And Na2CO3Raw material；
S2. weighed each raw material is mixed and is put into ball grinder, and be added and fitted according to the fluorescent powder total amount of required preparation
The dehydrated alcohol of amount；
S3. the ball grinder equipped with sample is placed in ball mill after ball milling with washes of absolute alcohol ball grinder and agate
Ball；
S4. sample is put into thermostatic drying chamber and is dried, and the resulting powder of drying is fully ground, then use tablet press machine
It is pressed into block；
S5. the block is placed in alumina crucible, is put into box high temperature sintering furnace and is sintered, that is, obtained described glimmering
Light powder.
Further, in step s3, the time of the ball milling is 10h；
In step s4, the drying temperature of the thermostatic drying chamber is 85 DEG C；
In step s5, the sintering temperature of the sintering furnace is 900 DEG C, sintering time 8h.
Detailed description of the invention
Fig. 1 is fluorescent powder NaLa0.7(MoO4)2-x(WO4)x:0.3Eu3+XRD spectrum；
Fig. 2 is the NaLa under 615nm monitoring0.7(MoO4)2-x(WO4)x:0.3Eu3+Excitation spectrum；
Fig. 3 is NaLa0.7(MoO4)2-x(WO4)x:0.3Eu3+Emission spectrum under 393nm excitation；
Fig. 4 is NaLa0.7(MoO4)2-x(WO4)x:0.3Eu3+Emission spectrum under 462nm excitation；
Fig. 5 is NaLa0.7(MoO4)2-x(WO4)x:0.3Eu3+Luminous intensity and WO4 2-The relationship of volume；
Fig. 6 is NaLa0.7(MoO4)2-x(WO4)x:0.3Eu3+Twilight sunset spectrum；
Fig. 7 is the chromaticity coordinates figure of fluorescent powder sample.
Specific embodiment
In order to make those skilled in the art that the present invention may be better understood, below with reference to embodiment to skill of the present invention
Art scheme further illustrates.
The preparation of fluorescent powder
The present embodiment prepares NaLa using high temperature solid-state method0.7(MoO4)2-x(WO4)x:0.3Eu3+(x=0,0.5,1,1. 5,
2) block red fluorescence powder.Step are as follows:
S1. La is weighed by certain stoichiometric ratio2O3(A.R.)、MoO3(A.R.), high-purity Eu2O3(99.9%), WO3
(A.R.) and Na2CO3(A.R.)；
S2. weighed each raw material is mixed and is put into ball grinder, and be added and fitted according to the fluorescent powder total amount of required preparation
The dehydrated alcohol of amount；
S3. will be placed in ball mill equipped with the ball grinder of sample, after ball milling 10h with washes of absolute alcohol ball grinder and
Agate ball；
S4. sample is put into 85 DEG C of thermostatic drying chambers and dries 6h, and the resulting powder of drying is fully ground, then uses
Tablet press machine is pressed into block；
S5. the block is placed in alumina crucible, is put into 900 DEG C of sintering 8h in box high temperature sintering furnace, that is, obtains
The fluorescent powder.
The XRD analysis of fluorescent powder
Fig. 1 is NaLa0.7(MoO4)2-x(WO4)x:0.3Eu3+The XRD spectrum of fluorescent powder.As can be seen from Figure 1, work as x=
When 1, the diffraction maximum and JCPDS No.24-1103 (NaLa (MoO of sample4)2) standard card is completely the same, without other miscellaneous phases
In the presence of illustrating WO4 2-It introduces there is no change phase structure, obtained product NaLa0.7(MoO4)(WO4): 0.3Eu3+With compared with
Good phase purity.As x=2, the diffraction maximum and JCPDS No.79-1118 (NaLa (MoWO of sample4)2) standard card is complete
Unanimously, NaLa0.7 (WO has been synthesized4)2:0.3Eu3+Phase.
The excitation spectrum of fluorescent powder
Fig. 2 is the NaLa for being sintered 8h at 900 DEG C and obtaining0.7(MoO4)2-x(WO4)x:0.3Eu3+Excitation spectrum, with 615nm
As monitoring wavelength.Known to being analyzed to sample, in sample NaLa0.7(MoO4)2:0.3Eu3+Middle introducing WO4 2-Replace part
MoO4 2-There is no the shape for changing sample excitation spectrum and peak positions, and only luminous intensity changes.As shown in Figure 2,
The excitation spectrum of sample is made of broadband and several spike two parts, and the excitation band near 300nm is a broadband, real
It is Eu in matter3+-O2+Charge transfer band and Mo6+-O2+Or W6+-O2+Charge-transfer band composition.Between 358~545nm
Excitation peak be to belong to activator Eu3+F → f transition absorption, wherein be located at 393nm at peak group be Eu3+'s7F0-5L6Jump
It moves, the excitation peak group at 462nm belongs to7F0→5D2Transition, the excitation peak group at 535nm belong to7F0→5D1Transition.
As can be seen from Figure 2, sample is in NaLa0.7(MoO4)2:0.3Eu3+Middle addition WO4 2-Afterwards, the absorption intensity at 462nm is high
At 393nm, illustrate W6+Addition so that the secondary crystal structure of the centre of luminescence changes, so that energy be made to shift.It is real
It tests and shows: respectively with 393nm black light and 462nm excited by visible light sample, Eu3+Transmitting peak type it is essentially the same, mainly by
Near 590nm5D0→7F1Electric dipole transition composition near magnetic dipole transition and 616nm, wherein with the strong light at 615nm
Degree is maximum.
The emission spectrum of fluorescent powder
Fig. 3 and Fig. 4 is sample NaLa0.7(MoO4)2-x(WO4)x:0.3Eu3+(x=0,0.5,1,1.5,2) respectively close purple
Emission spectrum under outer 393nm and blue light 462nm excitation.The emission spectrum of sample is by several groups of spikes between 585~630nm
Composition, is Eu3+F-f transition characteristics spectral line, be belonging respectively to Eu3+The different initial states of ion5D0To final state7FJ(J=0,1,2,
3,4) transition.Peak positioned at 590nm is due to Eu3+Magnetic dipole transition5D0→7F1Cause, is located at 611nm and 615nm
Peak be due to Eu3+Electric dipole5D0→7F2Transition causes.5D0→7F2Transition is better than5D0→7F1, the wherein hair at 615nm
It is most strong to penetrate peak.As figure shows, in NaLa0.7(MoO4)2-x(WO4)x: 0.3Eu3+Middle part Mo6+And W6+Occupy Mo jointly6+'s
Case.Sample uses the excitation of 393nm and 462nm wavelength all from Eu respectively3+'s7F0→5L6、7F0→5D2Transition, Eu3+It is logical
It crosses relaxation and transfers energy into low excited state5D0, then pass through Eu again3+'s5D0→7FJ(J=0,1,2,3,4) transition generates
Feux rouges.And the energy transfer of charge-transfer band is mainly Eu3+-O2+With
Mo6+-O2+/W6+-O2+O in charge transfer band2+2p track on electronics transit to Eu respectively3+And Mo6+/W6+'s
To generate energy transfer on unoccupied orbital.But in O2+-Mo6+/W6+Charge migration during, the migration of only part is logical
Relaxation transition in the form of thermal energy radiation is crossed, energy adjourns Eu by noradiative transition3+Excitation state5D0Energy level, to emit red
Light；Rest part is that energy is directly passed to by relaxation
Eu3+'s5H3Energy level.Therefore, do not see WO in figs. 3 and 44 2-And MoO4 2-Corresponding emission peak, only
See in Fig. 2 by Mo6+-O2+Or W6+-O2+And the characteristic peak generated, so that it is to pass through Eu that explanation, which shines,3+Non-radiative energy
Order transition and generate.
Fig. 5 is NaLa0.7(MoO4)2-x(WO4)x: 0.3Eu3+Sample respectively 393nm and 462nm excitation under strong light
Spend change curve.As seen from Figure 5, luminous intensity of the sample under 393nm and 462nm excitation is with WO4 2-The change of concentration
Change trend is similar, is all with WO4 2-The increase of concentration and increase.Work as W6+Replace Mo6+Ratio be 1 when, luminous intensity
Reach maximum value.It can be seen that W6+Doping can effectively improve the luminous intensity of fluorescent powder, this may be because of Eu3+Phase between ion
Interaction is changing, Eu3+-O2+And Mo6+-O2+/W6+-O2+Energy transfer can effectively reach Eu3+The centre of luminescence, to make
Luminous intensity increases.However work as WO4 2-Concentration when continuing growing, the luminous intensity of sample reduces instead.In addition, from Fig. 5
It is also seen that WO4 2-Introducing to sample 393nm excitation under luminous intensity the no 462nm of influence it is obvious.
The twilight sunset spectrum of fluorescent powder
For in sample NaLa0.7(MoO4)2: 0.3Eu3+Middle introducing W6+Resulting NaLa0.7(MoO4)2-x(WO4)x:
0.3Eu3+, from excitation spectrum, it can be seen that, the excitation of 393nm and 462nm can make sample issue feux rouges at 615nm, use
Red twilight sunset can be obtained after stopping in 254nm ultraviolet excitation, this phenomenon illustrates that the fluorescent powder has afterglow property.Use 254nm
Ultraviolet light, by Eu3+From O2+-Eu3+Charge transfer band excitation enters conduction band, and electronics moves freely in conduction band, and a part returns to
Eu3+Excitation state, to obtain recombination luminescence；Remaining electronics is captured by the trap near conduction band.After excitation stops, falling into
Electronics in trap is discharged back into conduction band, and a part returns to Eu3+Excitation state, to generate red twilight sunset.As can be seen from Figure 6, sample
Product twilight sunset spectrum is Eu3+'s5D0-7FJ(J=0,1,2,3,4) transition transmitting and generate, main peak is located at 615nm.
The chromaticity coordinates of fluorescent powder is analyzed
We calculate sample NaLa0.7(MoO4)2-x(WO4)x: 0.3Eu3+Under 393nm and 462nm ultraviolet excitation
Chromaticity coordinates value.By the chromaticity coordinates figure of Fig. 7 as can be seen, fluorescent powder NaLa0.7(MoO4)(WO4): 0.3Eu3+Colour code value ratio
NaLa0.7(MoO4)2: 0.3Eu3+Closer to the standard value of National Television System Committee (NTSC), illustrate to introduce W6+
Improve the excitation purity of sample.
The explanation of embodiments above is merely used to help understand method and its core concept of the invention.It should refer to
It out, for those skilled in the art, without departing from the principle of the present invention, can also be to this hair
Bright some improvement and modification can also be carried out, and these improvements and modifications also fall within the scope of protection of the claims of the present invention.
Claims (9)
1. one kind can be by ultraviolet light, black light or blue light activated red fluorescence powder, it is characterised in that: the change of the fluorescent powder
Formula are as follows: NaLa0.7(MoO4)2-x(WO4)x:0.3Eu3+, wherein x=0,0.5,1,1.5,2.
2. red fluorescence powder according to claim 1, it is characterised in that: the fluorescent powder can be by the black light of 393nm
It is excited with the blue light of 462nm, emission spectrum is made of the multiple groups spike between 585-630nm, wherein shining at 615nm
Maximum intensity.
3. red fluorescence powder according to claim 1, it is characterised in that: the fluorescent powder can improve hair by introducing wolframic acid
Luminous intensity.
4. red fluorescence powder according to claim 3, it is characterised in that: the fluorescent powder is under 393nm and 462nm excitation
Luminous intensity with WO4 2-The increase of concentration and increase, and work as W6+Replace Mo6+Doping ratio be 1 when, sample shine
Maximum intensity, and feux rouges excitation purity is best.
5. red fluorescence powder according to claim 1, it is characterised in that: the fluorescent powder is stopped with 254nm ultraviolet excitation
Red twilight sunset can be obtained after only.
6. a kind of preparation method for being used to prepare the described in any item red fluorescence powders of claim 1-5, it is characterised in that: including
Following steps:
S1. La is weighed2O3、MoO3、Eu2O3、WO3、Na2CO3Raw material；
S2. weighed each raw material is mixed and is put into ball grinder, and is suitable according to the addition of the fluorescent powder total amount of required preparation
Dehydrated alcohol；
S3. the ball grinder equipped with sample is placed in ball mill after ball milling with washes of absolute alcohol ball grinder and agate ball；
S4. sample is put into thermostatic drying chamber and is dried, and the resulting powder of drying is fully ground, then be pressed into block with tablet press machine
Body；
S5. the block is placed in alumina crucible, is put into box high temperature sintering furnace and is sintered, that is, obtain the fluorescent powder.
7. the preparation method according to claim 6, it is characterised in that: in step s3, the time of the ball milling is 10h.
8. the preparation method according to claim 6, it is characterised in that: in step s4, the drying of the thermostatic drying chamber
Temperature is 85 DEG C, and drying time is 6h.
9. the preparation method according to claim 6, it is characterised in that: in step s5, the sintering temperature of the sintering furnace
It is 900 DEG C, sintering time 8h.
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Application publication date: 20190101 |