CN104212442A - Preparation method of fluorescent material used for orange-yellow-color LED - Google Patents
Preparation method of fluorescent material used for orange-yellow-color LED Download PDFInfo
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- CN104212442A CN104212442A CN201410352422.5A CN201410352422A CN104212442A CN 104212442 A CN104212442 A CN 104212442A CN 201410352422 A CN201410352422 A CN 201410352422A CN 104212442 A CN104212442 A CN 104212442A
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- 239000000463 material Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 17
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 abstract description 25
- 230000008569 process Effects 0.000 abstract description 19
- 238000002156 mixing Methods 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 5
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 2
- 150000002910 rare earth metals Chemical class 0.000 abstract description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 abstract 2
- 230000002829 reductive effect Effects 0.000 abstract 2
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 238000005245 sintering Methods 0.000 abstract 1
- 239000006104 solid solution Substances 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 13
- 230000008859 change Effects 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000000376 reactant Substances 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000003746 solid phase reaction Methods 0.000 description 4
- 238000010671 solid-state reaction Methods 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 238000003836 solid-state method Methods 0.000 description 2
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical group O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 208000011117 substance-related disease Diseases 0.000 description 1
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- Luminescent Compositions (AREA)
Abstract
The invention discloses a preparation method of a fluorescent material used for an orange-yellow-color LED and belongs to the technical field of rare earth luminescent material. The fluorescent material used for the orange-yellow-color LED is a solid solution and a chemical formula of the fluorescent material is Sr3SiO5:Eu<2+>. The preparation method comprises following steps: (1) uniformly mixing raw materials including SrCO3, SiO2, Eu2O3 and NH4F; (2) performing a piece-pressing process to the uniformly mixed raw materials through a powder piece-pressing process to obtain a piece-pressed mixed material; and (3) finally placing the piece-pressed mixed material in a crucible, performing a sintering process under a reductive atmosphere at 1250-1350 DEG C for 3-5h, cooling the sintered material to room temperature under the reductive atmosphere, and performing a grinding process to obtain an Sr3SiO5:Eu<2+> single phase. The method is low in cost and simple in processes. By means of the preparation method, generation of an impurity phase, Sr2SiO4, is avoided during the synthetic process of the fluorescent material. Through treatment in the preparation method, a luminescent intensity of the LED fluorescent material is significantly increased on the basis of without influence of an initial luminance of the LED fluorescent material.
Description
Technical field
The present invention relates to a kind of preparation method of orange-yellow LED fluorescent material, belong to rare earth luminescent material technical field.
Background technology
Ya chemical company takes the lead in breaking through in blue GaN base LED technology for 1993, and very fast industrialization, developed white light LEDs in 1996, within 1998, push to market, cause insider and pay close attention to greatly.Compared with conventional illumination sources, white light LEDs has many advantages, as: volume is little, less energy consumption, response is fast, the life-span is long, pollution-free etc.The plurality of advantages of white light LEDs, makes its application in daily life increasing, as background illumination, traffic lights, total colouring and general lighting etc., has huge following illumination market and remarkable Energy-saving Perspective.The major programme realizing white light LEDs is at present: 1. the assembling of red, green, blue three-primary color LED chip is realized white light; 2. blue LED die and the Yellow light-emitting low temperature fluorescent material that effectively can be excited by blue light combine composition white light LEDs; 3. with sending out the LED chip of UV-light and near-ultraviolet light and effectively can being excited by UV-light and near-ultraviolet light and launch red, green, blue three primary colors fluorescent powder combination composition white light LEDs.In scheme 1, in use procedure, LED chip temperature raises, meeting appearance light decay in various degree, but the light decay degree difference sending out the chip of red, green, blue is large, gained white light is consequently caused to be mixed white light, aberration is obvious, makes to assemble with three-primary color LED chip the application that LED is emitted white light and is restricted.Scheme 2 is applied relatively extensive, but institute lacks longwave optical component in emitting white light, and the glow color of device can change, the color poor repeatability of each LED with the change of fluorescent coating thickness, and colour rendering index is low.Rapidly, the color of its white light is only determined by fluorescent material used, and therefore LED institute color development coloured silk is more stable, and adjustable color, colour rendering index are high, is the main development direction of white light LEDs in scheme 3 development recently.At present, the LED three primary colors fluorescent powder that effectively can be excited by purple light, near-ultraviolet light is just widely studied.
Wherein, be that the luminescent material of matrix has that the prices of raw and semifnished materials are cheap, Technological adaptability is wide, synthesis temperature is moderate, product stability high with silicate systems, thus such matrix is extensively concerned.Within 2007, Japanese Lumi-tech company limited starts the Sr for white-light LED encapsulation
3siO
5: Eu
2+the sale of orange-yellow LED fluorescent material, its luminous efficiency is 1.5 times of current commercial YAG:Ce fluorescent material; And it can by 390nm to 480nm optical excitation, and utilizing emitted light is centrally located at 580nm place, excites scope wider than YAG:Ce, emission wavelength, closer to red light district, may be used for manufacturing warm white LED illumination device.But, utilize Sr prepared by high temperature solid-state method at present
3siO
5: Eu
2+all there is impurity phase Sr
2siO
4exist, due to Eu
2+be incorporated in different phase structures and can show different optical properties, thus have impact on Sr
3siO
5: Eu
2+orange-yellow LED luminescent properties.Thus the Sr of pure phase is synthesized
3siO
5: Eu
2+practical significance is extremely important.The solution of this problem is to Sr
3siO
5: Eu
2+application and study significant.
Summary of the invention
The object of this invention is to provide a kind of preparation method of orange-yellow LED fluorescent material, this preparation technology is simple, with low cost, and can obtain pure Sr
3siO
5: Eu
2+fluorescent material.
Orange-yellow LED fluorescent material of the present invention is sosoloid, and its chemical formula is Sr
3siO
5: Eu
2+, the average grain of product is 15-20 micron, and its principal phase structure belongs to tetragonal system.
What the present invention designed sinters by compressing tablet the Sr prepared
3siO
5: Eu
2+silicate fluorescent powder, in powder compressing machine, after 10MPa ~ 30MPa compressing tablet, can prepare pure Sr
3siO
5: Eu
2+orange-yellow LED fluorescent material.
Fluorescent material of the present invention adopts high temperature solid-state method synthesis, and concrete steps comprise as follows:
(1) by SrCO
3(99.99%): SiO
2(99.99%): Eu
2o
3(99.99%): NH
4f(99.99%) mol ratio is 3:1:0.05:0.05, precise is also mixed in agate mortar, to add purity be mass percent concentration be more than 98% alcohol grinding 20 ~ 40min make it mix, alcohol add-on is 80% ~ 120% of mixture volume;
(2) raw material mixed is carried out compressing tablet by powder compressing machine to it and obtain the compound after compressing tablet;
(3) compound after compressing tablet described in step (2) is put into crucible, logical reducing atmosphere sinters 3 ~ 5h at the temperature of 1250 DEG C ~ 1350 DEG C, and is cooled to room temperature under this reducing atmosphere, namely obtains Sr after grinding
3siO
5: Eu
2+single-phase, and inclusion-free phase Sr
2siO
4generate.
Pressure range 10MPa ~ the 30MPa of described pressed powder.
Described reducing atmosphere to be volume percent be 5% H
2be the N of 95% with volume percent
2mixed gas.
Inventive principle: no matter be Sr
2siO
4building-up process or Sr
3siO
5building-up process all belong to heterogeneous solid state reaction, such reaction in, the synthesis of compound generally occurs in phase boundary, for particulate state reactant, first reaction is undertaken by intergranular point of contact or face, follows and to be spread by product layer by reactant, reaction is continued.Therefore participate in the solid state reaction of reacting, contact is the prerequisite that chemical action and substance use occur between reactant.After form one deck product between two kinds of reaction particles, reaction is achieved depending on one or more reactants by the diffusion of product layer further, and this diffusion mobility can be undertaken by crystals lattice, surface, crystal boundary faceted crystal crack.With regard to Sr
3siO
5: Eu
2+building-up process, reaction process comprise three classes reaction:
：SrCO
3 → SrO +CO
2↑，
：2SrO + SiO
2 → Sr
2SiO
4，
：
3SrO + SiO
2→Sr
3SiO
5，
The decomposition of Strontium carbonate powder occurs in 800-1000 DEG C (process I); Subsequently, when temperature reaches the temperature range of about 1200 DEG C, Sr is reached
2siO
4: Eu
2+synthesis temperature, Sr
2siO
4: Eu
2+in this temperature range synthesis (process I); Raw material and crucible contact position can be regarded as the separation surface of two groups of materials, therefore Sr
2siO
4first can this separation surface synthesize.Work as Sr
2siO
4: Eu
2+after generation, it generates nitride layer and initial material can form new separation surface, and remaining reaction raw material has to diffuse through Sr
2siO
4: Eu
2+could at the enterprising single step reaction of separation surface after product layer.Solid state reaction process total in heterogeneous solid state reaction should comprise reactant and be diffused into phase boundary, carries out reacting and reaction product is removed from phase boundary in some cases, to Sr in phase boundary
2siO
4: Eu
2+building-up process, it is a slowest step that reactant is diffused into phase boundary, is namely the controlling unit of this process.When reaction product synthesis speed is subject to the diffusion control by reaction product layer, product layer thickness
xwith the time
tformula (1) can be passed through qualitatively calculate:
， （1）
Wherein
for reaction rate constant and by
determine.
qfor reaction activity; R is Avogadro constant,
tfor temperature of reaction.In temperature-rise period, pass through control process
reaction times
tor speed of reaction
kimpurity phase Sr can be controlled
2siO
4content.By increasing temperature rise rate, shorten the impurity phase Sr that about 1200 DEG C temperature ranges occur
2siO
4: Eu
2+generated time, greatly reduces impurity phase Sr equally
2siO
4volume fraction.And the sample of tabletted also makes powder particle be filled with hole while decreasing the area that raw material contacts with sidewall of crucible, rearranged position, atomic arrangement is tightr, causes raw material rate of diffusion to reduce, therefore, when temperature reaches 1200 DEG C, impurity phase Sr is made
2siO
4volume fraction greatly reduce.
The invention has the beneficial effects as follows: orange-yellow LED luminescent material prepared by the present invention is placed in atmosphere for a long time can not deliquescence, and phase structure can not change, chemical stability and thermostability high; The fluorescent material inclusion-free phase Sr prepared by this technique
2siO
4exist, this preparation method's technique is simple, with low cost.
Accompanying drawing explanation
Fig. 1 is the Sr that the embodiment of the present invention 1 prepares
3siO
5: Eu
2+the XRD figure spectrum of fluorescent material;
Fig. 2 is the Sr of the embodiment of the present invention 2 gained
3siO
5: Eu
2+fluorescent material photo;
Fig. 3 is the Sr that the embodiment of the present invention 3 prepares
3siO
5: Eu
2+the XRD figure spectrum after 24h placed by fluorescent material.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail, but protection scope of the present invention is not limited to described content.
Embodiment 1
The orange-yellow LED luminescent material of present embodiment is Sr
3siO
5: Eu
2+.Concrete preparation method is:
(1) by SrCO
3(99.99%), SiO
2(99.99%), Eu
2o
3(99.99%), NH
4f(99.99%) mol ratio is the ratio precise SrCO of 3:1:0.05:0.05
3, SiO
2, Eu
2o
3, NH
4f, mixing is placed in agate mortar and makes it mix, and in mixing process, add purity be mass percent is that 98% alcohol grinding 20min makes it mix, and alcohol add-on is 80% of mixture volume;
(2) raw material mixed is carried out compressing tablet by powder compressing machine to it and obtain the compound after compressing tablet (pressure of tabletting machine is 25MPa);
(3) compound after step (2) gained compressing tablet is put into crucible, (volume percent is the H of 5% to logical reducing atmosphere
2be the N of 95% with volume percent
2mixed gas), be rapidly heated (temperature rise rate is 40 DEG C/min), sinters 5h, and be cooled to room temperature at the temperature of 1250 DEG C under this reducing atmosphere, namely obtains pure orange-yellow LED fluorescent material Sr after grinding
3siO
5: Eu
2+, the luminescent material prepared is placed at ambient temperature can not deliquescence, and phase structure can not change, and inclusion-free phase Sr
2siO
4generate.The Sr that the present embodiment prepares
3siO
5: Eu
2+the XRD figure spectrum of fluorescent material as shown in Figure 1, can prepare pure Sr by the method for the invention as seen from the figure
3siO
5: Eu
2+single-phase.
Embodiment 2
The orange-yellow LED luminescent material of present embodiment is Sr
3siO
5: Eu
2+.Concrete preparation method is:
(1) by SrCO
3(99.99%), SiO
2(99.99%), Eu
2o
3(99.99%), NH
4f(99.99%) mol ratio is the ratio precise SrCO of 3:1:0.05:0.05
3, SiO
2, Eu
2o
3, NH
4f, mixing is placed in agate mortar and makes it mix, and in mixing process, add purity is that mass percent 98% alcohol grinding 25min makes it mix, and alcohol add-on is 90% of mixture volume;
(2) raw material mixed is carried out compressing tablet by powder compressing machine to it and obtain the compound after compressing tablet (pressure of tabletting machine is 15MPa);
(3) compound after step (2) gained compressing tablet is put into crucible, (volume percent is the H of 5% to logical reducing atmosphere
2be the N of 95% with volume percent
2mixed gas), be rapidly heated (temperature rise rate is 40 DEG C/min), sinters 3.5h, and be cooled to room temperature at the temperature of 1300 DEG C under this reducing atmosphere, namely obtains pure orange-yellow LED fluorescent material Sr after grinding
3siO
5: Eu
2+, the luminescent material prepared is placed at ambient temperature can not deliquescence, and phase structure can not change, and inclusion-free phase Sr
2siO
4generate.
The Sr of the present embodiment gained
3siO
5: Eu
2+as shown in Figure 2, (yellow powder is Sr to fluorescent material photo can to prepare pure yellow powder by embodiment 2 as seen from the figure
3siO
5phase, white powder is Sr
2siO
4phase), namely prepare pure Sr
3siO
5: Eu
2+single-phase.
Embodiment 3
The orange-yellow LED luminescent material of present embodiment is Sr
3siO
5: Eu
2+.Concrete preparation method is:
(1) by SrCO
3(99.99%), SiO
2(99.99%), Eu
2o
3(99.99%), NH
4f(99.99%) mol ratio is the ratio precise SrCO of 3:1:0.05:0.05
3, SiO
2, Eu
2o
3, NH
4f, mixing is placed in agate mortar and makes it mix, and in mixing process, add purity is that mass percent 99.9% alcohol grinding 30min makes it mix, and alcohol add-on is 100% of mixture volume;
(2) raw material mixed is carried out compressing tablet by powder compressing machine to it and obtain the compound after compressing tablet (pressure of tabletting machine is 30MPa);
(3) compound after step (2) gained compressing tablet is put into crucible, (volume percent is the H of 5% to logical reducing atmosphere
2be the N of 95% with volume percent
2mixed gas), be rapidly heated (temperature rise rate is 40 DEG C/min), sinters 4h, and be cooled to room temperature at the temperature of 1325 DEG C under this reducing atmosphere, namely obtains pure orange-yellow LED fluorescent material Sr after grinding
3siO
5: Eu
2+, the luminescent material prepared is placed at ambient temperature can not deliquescence, and phase structure can not change, and inclusion-free phase Sr
2siO
4generate.The Sr that the present embodiment prepares
3siO
5: Eu
2+xRD figure after 24h placed by fluorescent material is composed as shown in Figure 3: can prepare pure Sr by the present embodiment as seen from the figure
3siO
5: Eu
2+single-phase, and the long-time rear phase structure of placement can not change in atmosphere.
Embodiment 4
The orange-yellow LED luminescent material of present embodiment is Sr
3siO
5: Eu
2+.Concrete preparation method is:
(1) by SrCO
3(99.99%), SiO
2(99.99%), Eu
2o
3(99.99%), NH
4f(99.99%) mol ratio is the ratio precise SrCO of 3:1:0.05:0.05
3, SiO
2, Eu
2o
3, NH
4f, mixing is placed in agate mortar and makes it mix, and in mixing process, add purity is that mass percent 99% alcohol grinding 40min makes it mix, and alcohol add-on is 120% of mixture volume;
(2) raw material mixed is carried out compressing tablet by powder compressing machine to it and obtain the compound after compressing tablet (pressure of tabletting machine is 10MPa);
(3) compound after step (2) gained compressing tablet is put into crucible, (volume percent is the H of 5% to logical reducing atmosphere
2be the N of 95% with volume percent
2mixed gas), be rapidly heated (temperature rise rate is 40 DEG C/min), sinters 3h, and be cooled to room temperature at the temperature of 1350 DEG C under this reducing atmosphere, namely obtains pure orange-yellow LED fluorescent material Sr after grinding
3siO
5: Eu
2+, the luminescent material prepared is placed at ambient temperature can not deliquescence, and phase structure can not change, and inclusion-free phase Sr
2siO
4generate.
The Sr that the present embodiment prepares
3siO
5: Eu
2+fluorescent material fluorescent material under uv light irradiation sends pure orange coloured light, does not occur green emitting (Eu
2+at impurity phase Sr
2siO
4green light), prove to prepare pure Sr by the method for the invention
3siO
5: Eu
2+single-phase.
Claims (5)
1. a preparation method for orange-yellow LED fluorescent material, is characterized in that, specifically comprise the following steps:
(1) by raw material SrCO
3, SiO
2, Eu
2o
3, NH
4f mixes;
(2) raw material mixed is carried out compressing tablet by powder compressing machine to it and obtain the compound after compressing tablet;
(3) compound after compressing tablet described in step (2) is put into crucible, logical reducing atmosphere sinters 3 ~ 5h at the temperature of 1250 DEG C ~ 1350 DEG C, and is cooled to room temperature under this reducing atmosphere, namely obtains Sr after grinding
3siO
5: Eu
2+single-phase.
2. the preparation method of orange-yellow LED fluorescent material according to claim 1, is characterized in that: SrCO described in step (1)
3, SiO
2: Eu
2o
3: NH
4the mol ratio of F is 3:1:0.05:0.05.
3. the preparation method of orange-yellow LED fluorescent material according to claim 1, it is characterized in that: described in step (1), hybrid mode is for adding alcohol, fully 20 ~ 40min is ground in agate mortar, raw material is mixed, the mass percent concentration of described alcohol is more than 98%, and add-on is 80% ~ 120% of mixture volume.
4. the preparation method of orange-yellow LED fluorescent material according to claim 1, is characterized in that: the pressure range 10MPa ~ 30MPa of pressed powder described in step (2).
5. the preparation method of orange-yellow LED fluorescent material according to claim 1, is characterized in that: reducing atmosphere described in step (3) to be volume percent be 5% H
2be the N of 95% with volume percent
2mixed gas.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116395733A (en) * | 2023-03-28 | 2023-07-07 | 昆明理工大学 | CuAlO with adjustable optical property 2 Preparation method of powder material |
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