CN104212455B - A kind of Ce3+The garnet structure fluorescent material activated and its preparation method - Google Patents
A kind of Ce3+The garnet structure fluorescent material activated and its preparation method Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 118
- 239000002223 garnet Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims description 32
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 15
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 11
- 229910052788 barium Inorganic materials 0.000 claims abstract description 9
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 7
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 7
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 6
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 6
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 25
- 239000002994 raw material Substances 0.000 claims description 19
- 239000012298 atmosphere Substances 0.000 claims description 17
- 150000001875 compounds Chemical class 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 5
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 5
- 239000012467 final product Substances 0.000 claims description 5
- 241001025261 Neoraja caerulea Species 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000005538 encapsulation Methods 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 50
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 24
- 239000000395 magnesium oxide Substances 0.000 description 22
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 22
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 22
- 229910000420 cerium oxide Inorganic materials 0.000 description 20
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 20
- 239000000047 product Substances 0.000 description 19
- 239000000377 silicon dioxide Substances 0.000 description 19
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 18
- 239000011777 magnesium Substances 0.000 description 17
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 16
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 12
- 238000002441 X-ray diffraction Methods 0.000 description 12
- 238000000498 ball milling Methods 0.000 description 12
- 239000004570 mortar (masonry) Substances 0.000 description 12
- 229910052593 corundum Inorganic materials 0.000 description 11
- 239000010431 corundum Substances 0.000 description 11
- 238000013467 fragmentation Methods 0.000 description 11
- 238000006062 fragmentation reaction Methods 0.000 description 11
- 239000011575 calcium Substances 0.000 description 10
- 235000012239 silicon dioxide Nutrition 0.000 description 10
- 229960001866 silicon dioxide Drugs 0.000 description 10
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 9
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 8
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 7
- 238000007873 sieving Methods 0.000 description 7
- 229910000019 calcium carbonate Inorganic materials 0.000 description 6
- 238000000227 grinding Methods 0.000 description 6
- 229910002651 NO3 Inorganic materials 0.000 description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 5
- 229910052791 calcium Inorganic materials 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 229910000018 strontium carbonate Inorganic materials 0.000 description 5
- BEDFIBPNPHRGDO-UHFFFAOYSA-N yttrium;hydrate Chemical compound O.[Y] BEDFIBPNPHRGDO-UHFFFAOYSA-N 0.000 description 5
- 238000011068 loading method Methods 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- 238000000695 excitation spectrum Methods 0.000 description 3
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 description 3
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 229910052727 yttrium Inorganic materials 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 2
- 239000004567 concrete Substances 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910002492 Ce(NO3)3·6H2O Inorganic materials 0.000 description 1
- -1 Ion-activated yttrium aluminum garnet Chemical class 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- CQGVSILDZJUINE-UHFFFAOYSA-N cerium;hydrate Chemical compound O.[Ce] CQGVSILDZJUINE-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005090 crystal field Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- XMHIUKTWLZUKEX-UHFFFAOYSA-N hexacosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O XMHIUKTWLZUKEX-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 description 1
- YXEUGTSPQFTXTR-UHFFFAOYSA-K lanthanum(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[La+3] YXEUGTSPQFTXTR-UHFFFAOYSA-K 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
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- Luminescent Compositions (AREA)
Abstract
The present invention discloses a kind of Ce3+The garnet structure fluorescent material activated, chemical expression is: Mg2-aAaY2-x-bBbM2N2O12:xCe3+In formula: A is one or more the combination in Ba, Sr, Ca, B is one or more the combination in Gd, La, Sc, M is the combination of one or both arbitrary proportions in Al, Ga, N is the combination of one or both arbitrary proportions in Si, Ge, x, a, b are respective molar fraction, their span is: 0.01≤x≤0.12,0≤a≤0.2,0≤b≤0.2. Fluorescent material provided by the invention wavelength be 460nm blue-light excited under, it is possible to sending wavelength region is 500 to the orange light of 750nm, it is possible to be applied in white light LEDs.
Description
Technical field
The invention belongs to luminescent material technical field, it is specifically related to be applied to the fluorescent material of semiconductor lighting, especially relate to a kind of effectively can being excited by blue-light LED chip and launch fluorescent material and its preparation method of orange light.
Background technology
In the manufacture method of white light LEDs, the method applying yellow fluorescent powder on blue InGaN chip due to its method simple, with low cost, and the LED component efficiency height obtained, and receive maximum concerns. In the yellow fluorescent powder used, Ce3+Ion-activated yttrium aluminum garnet (Y3A15O12:Ce3+, it is called for short YAG:Ce3+) owing to blue light can be absorbed efficiently and converts thereof into yellow light, thus become commercial yellow fluorescent powder the most important at present. By InGaN chip composite Y AG:Ce3+The white light LEDs that fluorescent material is made, its efficiency more than 80lm/W, almost can match in excellence or beauty with the efficiency of luminescent lamp. But due to YAG:Ce3+In phosphor emission spectrum green composition too much and red composition very little, after blue-light LED chip compound, the white light of relative colour temperature (CCT) higher than 4500K can only be produced. This kind of white light, owing to tone is colder, color developing is poor, generally can only be used for outdoor lighting light source such as street lamp, headlight etc., and as interior lighting light source, thus should not seriously constrain the development of white light LEDs. The warm white LED that can produce CCT in 2500-3200K to manufacture, it is necessary at YAG:Ce3+Yellow fluorescent powder is mixed into (Sr, Ca) S:Eu2+、(Ba,Sr,Ca)2Si5N8:Eu2+、CaAlSiN3:Eu2+Etc. can by blue-light excited sulfide, nitride substrate red fluorescence powder. Although this kind of method can make up YAG:Ce to a certain extent3+The deficiency of fluorescent material, but also bring new problem: and being first that sulfide, nitride have its shortcoming separately, such as the former chemical stability is not good, and is harmful to by environment, and the preparation condition of the latter is very harsh, and cost is very high;Secondly, absorbing again due to emitted energy between different fluorescent material so that its glow color is unstable. Therefore, the LED yellow fluorescent powder of development of new becomes a popular problem.
In the design and chosen process of novel yellow fluorescent material, the garnet structure matrix that can produce strong crystal field is subject to the people's attention. 2006, Setlur etc. reported Ce3+The principal phase activated is the fluorescent material Lu of garnet structure2CaMg2Si3O12:Ce3+The characteristics of luminescence. Lu2CaMg2Si3O12:Ce3+The characteristics of luminescence of fluorescent material shows that garnet structure silicate is the excellent substrates of potential yellow light material. So far the silicate of the reported garnet structure utilizing solid reaction process to obtain is actually rare. Except Ce3+The Lu activated2CaMg2Si3O12Outside, only Ce3+The Ca activated3Sc2Si3O12。Lu2CaMg2Si3O12:Ce3+The transmitting main peak of fluorescent material is at 605nm. Quantum yield is 60%, by Lu2CaMg2Si3O12:Ce3+Encapsulating with blue-light LED chip, the white light colour temperature obtained is 3500K, but its color developing is lower, is only 76, it is easy to cause color deviation. And Ca3Sc2Si3O12:Ce3+The main peak of fluorescent material at 505nm, transmitting be green glow, cannot directly and blue chip combined transmit white light, it is necessary to just can access white light with red light fluorescent powder combination.
Summary of the invention
For the above-mentioned problems in the prior art, it is an object of the invention to provide a kind of novel emission wavelength relative to YAG:Ce3+Obvious red shift, white light LEDs cerium-ion activated garnet structure fluorescent material and its preparation method that preparation temperature is low.
The technical solution used in the present invention is:
A kind of Ce3+The garnet structure fluorescent material activated, it is characterised in that the chemical expression of described fluorescent material is:
Mg2-aAaY2-x-bBbM2N2O12:xCe3+
In formula: A is one or more the combination in Ba, Sr, Ca, B is one or more the combination in Gd, La, Sc, M is the combination of one or both arbitrary proportions in Al, Ga, N is the combination of one or both arbitrary proportions in Si, Ge, x, a, b are respective molar fraction, their span is: 0.01≤x≤0.12,0≤a≤0.2,0≤b≤0.2.
Further, it is preferable that 0.03≤x≤0.09.
In fluorescent material provided by the invention, a, b can be 0 separately, namely do not adulterate element A or B element. When a and b is 0 simultaneously, namely represent A and B that simultaneously do not adulterate in fluorescent material.
Further, A is preferably the mixing of ratio 1:0.5～1.5:0.5～1.5 of Ba, Sr or Ba, Sr, Ca amount of substance.
B is preferably La or Gd.
M is preferably Al, Ga or Al, the ratio of Ga amount of substance is the combination of 1:0.1～10.
N is preferably Si, Ge or Si, the ratio of Ge amount of substance is the combination of 1:0.1～10.
Further, it is preferable that the most basic structural formula of fluorescent material of the present invention is Mg2Y2-xM2N2O12:xCe3+, the performance of the composition adjustable fluorescent material of doping A, B ion and change M, N.
The present invention also provides the preparation method of described fluorescent material, and high temperature solid-state method can be adopted to prepare, and described method is: the chemical expression according to fluorescent material: Mg2-aAaY2-x-bBbM2N2O12:xCe3+In formula: A is one or more the combination in Ba, Sr, Ca, B is one or more the combination in Gd, La, Sc, M is the combination of one or both arbitrary proportions in Al, Ga, N is the combination of one or both arbitrary proportions in Si, Ge, and x, a, b are respective molar fraction, and their span is: 0.01≤x≤0.12,0≤a≤0.2,0≤b≤0.2;
Taking respectively containing the compound of each element in chemical expression as raw material, corresponding described raw material is taken by the molar ratio of element each in above-mentioned chemical expression, directly it is ground to obtain presoma with pressed powder, presoma is placed in reducing atmosphere, it is warming up to 900 DEG C～1350 DEG C roasting temperatures 1～5 time (preferably 1～2 time), obtains final product of roasting;Described temperature rise rate is generally 5 DEG C/min～20 DEG C/min, each roasting time is 5～24 hours, between every twice roasting, cool to room temperature carries out milled processed, last roasting carries out under reducing atmosphere, described reducing atmosphere is the nitrogen mixture containing 5-10v% hydrogen or the nitrogen mixture containing 5-10v% carbon monoxide, final product of roasting is through broken, levigate, size grading, and namely obtains described Ce through washing impurity-removing, oven dry3+The garnet structure fluorescent material activated.
Grinding of the present invention can carry out in agate mortar or ball mill.
The method of described size grading is one or more in settling process, method of sieving or air-flow method.
Final product of roasting, through broken, levigate, size grading, refers to and makes the particle size of sintered compact levigate with ball milling method again after adopting hand-crushed, through settling process, method of sieving or air-flow method classification, get the pressed powder that granularity is 3～10 microns.
Described washing impurity-removing, oven dry are successively by water, methanol wash, filter to isolate solid phase, in 100 DEG C～115 DEG C oven dry.
The raw material of described fluorescent material is the compound containing each element in chemical expression respectively, can choose the compound containing this element as raw material according to the various elements contained in chemical expression. Concrete, the raw material of described fluorescent material comprises compound containing Mg, Y, M, N, Ce separately, fluorescent material adulterates A or B time, then raw material also comprises the compound of each self-contained A or B.
More specifically, the described compound containing Mg, Ca, Sr or Ba is for containing each self-corresponding oxide compound of Mg, Ca, Sr or Ba, carbonate, oxyhydroxide or nitrate; Compound containing Al is in aluminum oxide, aluminium hydroxide or aluminum nitrate; Compound containing Y or Ce is containing each self-corresponding oxide compound of Y or Ce or nitrate; Compound containing Si is silicon-dioxide or water glass; Compound containing Ge, Gd, Ga or Sc is containing each self-corresponding oxide compound of Ge, Gd, Ga or Sc; Compound containing La is lanthanum trioxide, lanthanum nitrate, lanthanum hydroxide or Phosbloc.
Ce provided by the invention3+The garnet structure fluorescent material activated is a kind of at the blue-light excited fluorescent material issuing orange light.
Ce of the present invention3+The garnet structure fluorescent material activated can be applied in white light LEDs.
Concrete, the method for described application is, Ce3+The garnet structure fluorescent material activated and the encapsulation of blue-ray LED diode chip for backlight unit, for the preparation of white light LEDs.
Compared with prior art, the useful effect of the present invention is as follows:
1) the present invention is by adopting technique scheme, adds Ce3+Making the garnet structure fluorescent material that activator obtains, be a kind of type material being suitable for the white light LEDs application that blue-light LED chip excites, its sintering temperature is lower, energy-conservation than synthesis YAG:Ce (T=1400～1600 DEG C).
2) fluorescent material of the present invention can be absorbed in the blue light of 450nm to 500nm, therefore, it is possible to by wavelength be 450nm to 470nm blue light for InGaN effectively excite, the scope of emmission spectrum is 500nm to 750nm. More particularly, the present invention wavelength be 460nm blue-light excited under, the emission wavelength ranges of described garnet structure fluorescent material is 500 to 750nm, its main peak at about 601nm, with YAG:Ce3+Compare the about 60nm of red shift. Utilize the GaN base blue-ray LED basis light source that wavelength is 460nm to 470nm to excite, thus it is inspired orange light, after remaining blue light and orange yellow light mix, white light the present invention and YAG:Ce can be produced3+Comparing, its colour rendering index is higher, and colour temperature is lower.
Accompanying drawing explanation
Fig. 1 be the embodiment of the present invention 1 obtained mix Ce3+The excitation spectrum of garnet structure fluorescent material and emmission spectrum figure.
In figure: bold portion is exciting light spectrogram, dotted portion is emmission spectrum figure.
Fig. 2 be the embodiment of the present invention 1 obtained mix Ce3+The X-ray diffraction spectrogram of garnet structure fluorescent material.
Embodiment
With specific embodiment, the solution of the present invention is described further below, but protection scope of the present invention is not limited to this.
Embodiment 1:
Mg2Y1.97Al2Si2O12:0.03Ce3+The preparation of fluorescent material.
Preparation method is as follows:
Take 0.4030 gram of magnesium oxide (MgO), 1.1121 grams of yttrium oxide (Y respectively2O3), 0.6008 gram of silicon-dioxide (SiO2), 0.0258 gram of cerium oxide (CeO2), 0.5098 gram of aluminium sesquioxide (Al2O3), above material purity is all more than 99%. By above-mentioned raw materials mixture in agate mortar, after grinding evenly, loading in corundum crucible, taking the nitrogen mixture containing 5v% hydrogen as reducing atmosphere, temperature rise rate is 10 DEG C/min, with 900 DEG C of roastings 8 hours, naturally cool to room temperature, the sample of pre-burning is taken out and again grinds, then rise to temperature required (1350 DEG C) with the speed of 10 DEG C/min, constant temperature 8h, is cooled to room temperature. The sintered products obtained is after fragmentation, levigate with ball milling, method of sieving obtains granularity at the pressed powder of 3～10 microns, filter to isolate fluorescent material after washing with deionized water (30ml) and methyl alcohol (20ml) successively, dry in the baking oven of 120 DEG C and namely obtain fluorescent material product in 8 hours. This fluorescent material 460nm blue-light excited under emission wavelength between 500nm to 750nm, launch predominant wavelength 599nm. Chromaticity coordinates is (x=0.500, y=0.485).
What the present embodiment was obtained mixes Ce3+The excitation spectrum of garnet structure fluorescent material and emmission spectrum spectrogram as shown in Figure 1, wherein bold portion is excitation spectrum spectrogram (λ em=599nm), and dotted portion is emmission spectrum spectrogram (λ ex=460nm).
As can be seen from Figure 1, this fluorescent material 460nm blue-light excited under emission wavelength between 500nm to 750nm, launch predominant wavelength be respectively 599nm. Record its chromaticity coordinates for (x=0.500, y=0.485). This fluorescent material can blue-light excited by from 400nm to 500nm, be the new phosphors being suitable for the white light LEDs application that blue-light LED chip excites.
Fig. 2 be embodiment 1 obtained mix Ce3+The X-ray diffraction spectrogram of garnet structure fluorescent material, Fig. 2 is it may be seen that obtained fluorescent material is garnet structure. Embodiment 2:
Mg1.8Ba0.2Y1.97Al2Si2O12:0.03Ce3+The preparation of fluorescent material.
Preparation method is as follows:
Take 0.3627 gram of magnesium oxide (MgO), 0.1974 gram of barium carbonate (BaCO respectively3), 1.1121 grams of yttrium oxide (Y2O3), 0.6008 gram of silicon-dioxide (SiO2), 0.0258 gram of cerium oxide (CeO2), 0.5098 gram of three aluminum oxide (Al2O3), above material purity is all more than 99%. Above-mentioned raw materials mixture is ground in agate mortar after evenly and obtain presoma, the presoma obtained is placed in corundum crucible, using the nitrogen mixture of 5v% hydrogen as reducing atmosphere, in retort furnace, it is warming up to 900 DEG C with the speed of 10 DEG C/min, constant temperature 8h. The sample of pre-burning is taken out and again grinds, rise to temperature required (1340 DEG C) with the speed of 10 DEG C/min again, constant temperature 12h, it is cooled to room temperature, the sintered products obtained is after fragmentation, levigate with ball milling, and method of sieving obtains granularity at the pressed powder of 3～10 microns, filter to isolate fluorescent material after washing with deionized water (30ml) and methyl alcohol (20ml) successively, dry in the baking oven of 110 DEG C and namely obtain fluorescent material product in 12 hours.This fluorescent material 460nm blue-light excited under, transmitting main peak is 601nm, and emission wavelength is between 500nm to 750nm. Chromaticity coordinates is (x=0.523, y=0.468). This fluorescent material can blue-light excited by from 400nm to 500nm, be the new phosphors being suitable for the white light LEDs application that blue-light LED chip excites. The X-ray diffraction spectrogram of this fluorescent material and Fig. 2 are similar, are garnet structure. Embodiment 3:
Mg1.85Sr0.05Ca0.05Ba0.05Y1.94Al2Si2O12:0.06Ce3+The preparation of fluorescent material.
Preparation method is as follows:
Take 0.3728 gram of magnesium oxide (MgO), 0.0494 gram of barium carbonate (BaCO respectively3), 0.0369 gram of Strontium carbonate powder (SrCO3), 0.0250 gram of calcium carbonate (CaCO3), 3.7152 gram of six nitric hydrate yttrium (Y (NO3)3·6H2O), 0.6008 gram of silicon-dioxide (SiO2), 0.0516 gram of cerium oxide (CeO2), 0.3900 gram of aluminium hydroxide (Al (OH)3), above material purity is all more than 99%. By above-mentioned raw materials mixture in agate mortar, after grinding evenly, loading in corundum crucible, taking the nitrogen mixture containing 5v% hydrogen as reducing atmosphere, temperature rise rate is 10 DEG C/min, is raised to 900 DEG C, and then constant temperature 8 hours, are cooled to room temperature. The sample of pre-burning is taken out and again grinds, rise to temperature required (1350 DEG C) with the speed of 5 DEG C/min again, constant temperature 8h, it is cooled to room temperature, the sintered products obtained is after fragmentation, levigate with ball milling, and method of sieving obtains granularity at the pressed powder of 3～10 microns, filter to isolate fluorescent material after washing with deionized water (30ml) and methyl alcohol (20ml) successively, dry in the baking oven of 110 DEG C and namely obtain fluorescent material product in 10 hours. This fluorescent material 460nm blue-light excited under emission wavelength between 500nm to 750nm, transmitting predominant wavelength is 602nm. Chromaticity coordinates is (x=0.519, y=0.472). This fluorescent material can blue-light excited by from 400nm to 500nm, be the new phosphors being suitable for the white light LEDs application that blue-light LED chip excites. The X-ray diffraction spectrogram of this fluorescent material and Fig. 2 are similar, are garnet structure.
Embodiment 4:
Mg2Y1.97Ga2Si2O12:0.03Ce3+The preparation of fluorescent material.
Preparation method is as follows:
Take 0.4030 gram of magnesium oxide (MgO), 1.8863 gram of six nitric hydrate yttrium (Y (NO respectively3)3·6H2O), 0.6008 gram of silicon-dioxide (SiO2), 0.0651 gram of six nitric hydrate cerium (Ce (NO3)3·6H2O), 0.9372 gram of gallium oxide (Ga2O3), above material purity is all more than 99%. By above-mentioned raw materials mixture in agate mortar, after grinding evenly, load in corundum crucible, taking the nitrogen mixture containing 5v% carbon monoxide as reducing atmosphere, temperature rise rate is 10 DEG C/min, with 900 DEG C of roastings 8 hours, it is cooled to room temperature, the sample of pre-burning is taken out and again grinds, then rise to temperature required (1250 DEG C) with the speed of 10 DEG C/min, constant temperature 8h, it is cooled to room temperature, again grind, then rise to temperature required (1300 DEG C) with the speed of 10 DEG C/min, constant temperature 10h. The sintered products obtained is after fragmentation, levigate with ball milling, method of sieving obtains granularity at the pressed powder of 3～10 microns, respectively wash twice with deionized water (30ml) and methyl alcohol (20ml) successively, finally filter to isolate fluorescent material, dry in the baking oven of 110 DEG C and namely obtain fluorescent material product in 15 hours. This phosphor emission wavelength light is between 500nm to 750nm, and transmitting predominant wavelength is 610nm, chromaticity coordinates (x=0.519, y=0.471). This fluorescent material can blue-light excited by from 400nm to 500nm, be the new phosphors being suitable for the white light LEDs application that blue-light LED chip excites.The X-ray diffraction spectrogram of this fluorescent material and Fig. 2 are similar, are garnet structure.
Embodiment 5:
Mg2Y1.91Al2Ge2O12:0.09Ce3+The preparation of fluorescent material.
Preparation method is as follows:
Take 0.4030 gram of magnesium oxide (MgO), 1.0782 grams of yttrium oxide (Y respectively2O3), 0.0774 gram of cerium oxide (CeO2), 0.5098 gram of three aluminum oxide (Al2O3), 1.0464 grams of germanium oxide (GeO2), above material purity is all more than 99%. Being ground in agate mortar by above-mentioned raw materials mixture after evenly, load in corundum crucible, taking the nitrogen mixture containing 5v% hydrogen as reducing atmosphere, temperature rise rate is 10 DEG C/min, with 900 DEG C of roastings 8 hours, is cooled to room temperature. The sample of pre-burning is taken out and again grinds, then rise to temperature required (1300 DEG C) with the speed of 10 DEG C/min, constant temperature 15h, it is cooled to room temperature, the sintered products obtained is after fragmentation, levigate with ball milling, and screening obtains granularity at the solid powder fluorescence powder of 3～10 microns. The emission wavelength of this fluorescent material is between 500nm to 750nm, and transmitting predominant wavelength is 608nm, and chromaticity coordinates is (x=0.509, y=0.481). This fluorescent material can blue-light excited by from 400nm to 500nm, be the new phosphors being suitable for the white light LEDs application that blue-light LED chip excites. The X-ray diffraction spectrogram of this fluorescent material and Fig. 2 are similar, are garnet structure.
Embodiment 6:
Mg2Y1.88La0.05Al2Si2O12:0.07Ce3+The preparation of fluorescent material.
Preparation method is as follows:
Take 0.4030 gram of magnesium oxide (MgO), 3.6003 gram of six nitric hydrate yttrium (Y (NO respectively3)3·6H2O), 0.6008 gram of silicon-dioxide (SiO2), 0.0602 gram of cerium oxide (CeO2), 0.5098 gram of three aluminum oxide (Al2O3), 0.0407 gram of lanthanum sesquioxide (La2O3), above material purity is all more than 99%. By above-mentioned raw materials mixture in agate mortar, after grinding evenly, loading in corundum crucible, taking the nitrogen mixture containing 5v% hydrogen as reducing atmosphere, temperature rise rate is 10 DEG C/min, with 900 DEG C of roastings 8 hours, it is cooled to room temperature, the sample of pre-burning is taken out and again grinds, then rise to temperature required (1350 DEG C) with the speed of 10 DEG C/min, constant temperature 8h, is cooled to room temperature. The sintered products obtained is after fragmentation, levigate with ball milling, method of sieving obtains granularity at the pressed powder of 3～10 microns, respectively wash twice with deionized water (30ml) and methyl alcohol (20ml) successively, finally filter to isolate fluorescent material, dry in the baking oven of 100 DEG C and namely obtain fluorescent material product in 20 hours. The emission wavelength of this fluorescent material under 460nm is blue-light excited is between 500nm to 750nm, and transmitting predominant wavelength is 601nm, and chromaticity coordinates is (x=0.508, y=0.482). This fluorescent material can blue-light excited by from 400nm to 500nm, be the new phosphors being suitable for the white light LEDs application that blue-light LED chip excites. The X-ray diffraction spectrogram of this fluorescent material and Fig. 2 are similar, are garnet structure.
Embodiment 7
Mg2Y1.87La0.1Al2Si1.8Ge0.2O12:0.03Ce3+The preparation of fluorescent material.
Preparation method is as follows:
Take 0.4030 gram of magnesium oxide (MgO), 1.7906 grams of yttrium oxide (Y respectively2O3), 0.5407 gram of silicon-dioxide (SiO2), 0.0258 gram of cerium oxide (CeO2), 0.5098 gram of three aluminum oxide (Al2O3), 0.0814 gram of lanthanum sesquioxide (La2O3), 0.1046 gram of germanium oxide (GeO2), above material purity is all more than 99%. Above-mentioned raw materials mixture is ground in agate mortar after evenly, load in corundum crucible, taking the nitrogen mixture containing 5v% carbon monoxide as reducing atmosphere, temperature rise rate is 5 DEG C/min, with 900 DEG C of roastings 8 hours, is cooled to room temperature, the sample of pre-burning is taken out and again grinds, rising to temperature required (1320 DEG C) with the speed of 5 DEG C/min, constant temperature 15h, is cooled to room temperature again.Get after sintered product grinds and heat up again, by above-mentioned roasting condition roasting 2 times, the sintered products obtained is levigate with ball milling after fragmentation, settling process obtains granularity at the pressed powder of 3～10 microns, respectively wash twice with deionized water (30ml) and methyl alcohol (20ml) successively, finally filter to isolate fluorescent material, dry in the baking oven of 110 DEG C and namely obtain fluorescent material product in 20 hours. The emission wavelength of this fluorescent material under 460nm is blue-light excited is between 500nm to 750nm, and transmitting predominant wavelength is 604nm, covers whole visible-range. Chromaticity coordinates is (x=0.508, y=0.482). This fluorescent material can blue-light excited by from 400nm to 500nm, be the new phosphors being suitable for the white light LEDs application that blue-light LED chip excites. The X-ray diffraction spectrogram of this fluorescent material and Fig. 2 are similar, are garnet structure.
Embodiment 8:
Mg2Y1.90Gd0.05Al2Si2O12:0.05Ce3+The preparation of fluorescent material.
Preparation method is as follows:
Take 0.4030 gram of magnesium oxide (MgO), 1.0726 grams of yttrium oxide (Y respectively2O3), 0.6008 gram of silicon-dioxide (SiO2), 0.0430 gram of cerium oxide (CeO2), 0.5098 gram of three aluminum oxide (Al2O3), 0.0453 gram of Gadolinium trioxide (Gd2O3), above material purity is all more than 99%. By above-mentioned raw materials mixture in agate mortar, after grinding evenly, loading in corundum crucible, taking the nitrogen mixture containing 5v% carbon monoxide as reducing atmosphere, temperature rise rate is 10 DEG C/min, with 900 DEG C of roastings 8 hours, it is cooled to room temperature, the sample of pre-burning is taken out and again grinds, then rise to temperature required (1350 DEG C) with the speed of 5 DEG C/min, constant temperature 8h, is cooled to room temperature. The sintered products obtained is after fragmentation, levigate with ball milling, settling process obtains granularity at the pressed powder of 3～10 microns, respectively wash twice with deionized water (30ml) and methyl alcohol (20ml) successively, finally filter to isolate fluorescent material, dry in the baking oven of 110 DEG C and namely obtain fluorescent material product in 20 hours. The emission wavelength of this fluorescent material under 460nm is blue-light excited is between 500nm to 750nm, and transmitting predominant wavelength is 592nm, covers whole visible-range. Chromaticity coordinates is (x=0.481, y=0.496). This fluorescent material can blue-light excited by from 400nm to 500nm, be the new phosphors being suitable for the white light LEDs application that blue-light LED chip excites. The X-ray diffraction spectrogram of this fluorescent material and Fig. 2 are similar, are garnet structure.
Embodiment 9:
Mg1.8Ba0.2Y1.87Gd0.1Al2Si2O12:0.03Ce3+The preparation of fluorescent material.
Preparation method is as follows:
Take 0.3627 gram of magnesium oxide (MgO), 0.1974 gram of barium carbonate (BaCO3), 1.0557 grams of yttrium oxide (Y respectively2O3), 0.6008 gram of silicon-dioxide (SiO2), 0.0258 gram of cerium oxide (CeO2), 0.5098 gram of three aluminum oxide (Al2O3), 0.0906 gram of Gadolinium trioxide (Gd2O3), above material purity is all more than 99%. Being ground in agate mortar by above-mentioned raw materials mixture after evenly, load in corundum crucible, taking the nitrogen mixture containing 5v% hydrogen as reducing atmosphere, temperature rise rate is 10 DEG C/min, with 900 DEG C of roastings 8 hours, is cooled to room temperature. The sample of pre-burning is taken out and again grinds, rise to temperature required (1350 DEG C) with the speed of 10 DEG C/min again, constant temperature 8h, the sample burnt is ground again, then rises to temperature required (1350 DEG C) with the speed of 10 DEG C/min, constant temperature 8h, it is cooled to room temperature, the sintered products obtained is after fragmentation, levigate with ball milling, and screening obtains granularity at the solid powder fluorescence powder of 3～10 microns. The emission wavelength of this fluorescent material is between 500nm to 750nm, and transmitting predominant wavelength is 608nm, and chromaticity coordinates is (x=0.481, y=0.496 colour rendering index Ra=91.This fluorescent material can blue-light excited by from 400nm to 500nm, be the new phosphors being suitable for the white light LEDs application that blue-light LED chip excites. The X-ray diffraction spectrogram of this fluorescent material and Fig. 2 are similar, are garnet structure.
Embodiment 10:
Mg1.85Sr0.05Ca0.05Ba0.05Y1.77Gd0.2Al2Si2O12:0.03Ce3+The preparation of fluorescent material.
Preparation method is as follows:
Take 0.3729 gram of magnesium oxide (MgO), 0.0494 gram of barium carbonate (BaCO3), 0.0369 gram of Strontium carbonate powder (SrCO respectively3), 0.0250 gram of calcium carbonate (CaCO3), 2.9914 gram of six nitric hydrate yttrium (Y (NO3)3·6H2O), 0.6008 gram of silicon-dioxide (SiO2), 0.0258 gram of cerium oxide (CeO2), 0.5098 gram of three aluminum oxide (Al2O3), 0.1812 gram of Gadolinium trioxide (Gd2O3), above material purity is all more than 99%. Being ground in agate mortar by above-mentioned raw materials mixture after evenly, load in corundum crucible, taking the nitrogen mixture containing 5v% hydrogen as reducing atmosphere, temperature rise rate is 10 DEG C/min, with 900 DEG C of roastings 8 hours, is cooled to room temperature. The sample of pre-burning is taken out and again grinds, then rise to temperature required (1340 DEG C) with the speed of 5 DEG C/min, constant temperature 10h, it is cooled to room temperature, the sintered products obtained is after fragmentation, levigate with ball milling, and screening obtains granularity at the solid powder fluorescence powder of 3～10 microns. The emission wavelength of this fluorescent material is between 500nm to 750nm, and transmitting predominant wavelength is 608nm, and chromaticity coordinates is (x=0.481, y=0.495). This fluorescent material can blue-light excited by from 400nm to 500nm, be the new phosphors being suitable for the white light LEDs application that blue-light LED chip excites. The X-ray diffraction spectrogram of this fluorescent material and Fig. 2 are similar, are garnet structure.
Embodiment 11:
Mg1.85Sr0.05Ca0.05Ba0.05Y1.77Gd0.2Al2Ge2O12:0.03Ce3+The preparation of fluorescent material.
Preparation method is as follows:
Take 0.3729 gram of magnesium oxide (MgO), 0.0494 gram of barium carbonate (BaCO respectively3), 0.0369 gram of Strontium carbonate powder (SrCO3), 0.0250 gram of calcium carbonate (CaCO3), 2.9914 gram of six nitric hydrate yttrium (Y (NO3)3·6H2O), 0.0258 gram of cerium oxide (CeO2), 0.5098 gram of three aluminum oxide (Al2O3), 0.1812 gram of Gadolinium trioxide (Gd2O3), 1.0464 grams of germanium oxide (GeO2), above material purity is all more than 99%. Being ground in agate mortar by above-mentioned raw materials mixture after evenly, load in corundum crucible, taking the nitrogen mixture containing 5v% hydrogen as reducing atmosphere, temperature rise rate is 10 DEG C/min, with 900 DEG C of roastings 8 hours, is cooled to room temperature. The sample of pre-burning is taken out and again grinds, then rise to temperature required (1310 DEG C) with the speed of 5 DEG C/min, constant temperature 10h, it is cooled to room temperature, the sintered products obtained is after fragmentation, levigate with ball milling, and screening obtains granularity at the solid powder fluorescence powder of 3～10 microns. The emission wavelength of this fluorescent material is between 500nm to 750nm, and transmitting predominant wavelength is 608nm, and chromaticity coordinates is (x=0.481, y=0.495). This fluorescent material can blue-light excited by from 400nm to 500nm, be the new phosphors being suitable for the white light LEDs application that blue-light LED chip excites. The X-ray diffraction spectrogram of this fluorescent material and Fig. 2 are similar, are garnet structure.
Claims (5)
1. a Ce3+The garnet structure fluorescent material activated, it is characterised in that the chemical expression of described fluorescent material is:
Mg2-aAaY2-x-bBbM2N2O12:xCe3+
In formula: A is one or more the combination in Ba, Sr, Ca, B is one or more the combination in Gd, La, Sc, M is the combination of one or both arbitrary proportions in Al, Ga, N is the combination of one or both arbitrary proportions in Si, Ge, x, a, b are respective molar fraction, their span is: 0.01≤x≤0.12,0≤a≤0.2,0≤b≤0.2.
2. fluorescent material as claimed in claim 1, it is characterised in that 0.03≤x≤0.09.
3. Ce as claimed in claim 13+The preparation method of the garnet structure fluorescent material activated, it is characterised in that described method is: the chemical expression according to fluorescent material: Mg2-aAaY2-x-bBbM2N2O12:xCe3+In formula: A is one or more the combination in Ba, Sr, Ca, B is one or more the combination in Gd, La, Sc, M is the combination of one or both arbitrary proportions in Al, Ga, N is the combination of one or both arbitrary proportions in Si, Ge, and x, a, b are respective molar fraction, and their span is: 0.01≤x≤0.12,0≤a≤0.2,0≤b≤0.2;
Taking respectively containing the compound of each element in chemical expression as raw material, corresponding described raw material is taken by the molar ratio of element each in above-mentioned chemical expression, directly it is ground to obtain presoma with pressed powder, presoma is placed in reducing atmosphere, it is warming up to 900 DEG C～1350 DEG C roasting temperatures 1～5 time, obtains final product of roasting; Each roasting time is 5～24 hours, between every twice roasting, cool to room temperature carries out milled processed, last roasting carries out under reducing atmosphere, described reducing atmosphere is the nitrogen mixture containing 5-10v% hydrogen or the nitrogen mixture containing 5-10v% carbon monoxide, final product of roasting is through broken, levigate, size grading, and namely obtains described Ce through washing impurity-removing, oven dry3+The garnet structure fluorescent material activated.
4. Ce as claimed in claim 1 or 23+The application of the garnet structure fluorescent material activated in white light LEDs.
5. apply as claimed in claim 4, it is characterised in that the method for described application is, Ce3+The garnet structure fluorescent material activated and the encapsulation of blue-ray LED diode chip for backlight unit, for the preparation of white light LEDs.
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| Tunable Color of Ce3+/Tb3+/Mn2+-Coactivated CaScAlSiO6 via Energy Transfer: A Single-Component Red/White-Emitting Phosphor;Wei Lü 等;《Inorg. Chem.》;20130227;第52卷;3007-3012 * |
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