CN103396794B - Eu<3+> activated sodium barium tungstate fluorescent powder, preparation method and application thereof - Google Patents
Eu<3+> activated sodium barium tungstate fluorescent powder, preparation method and application thereof Download PDFInfo
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- CN103396794B CN103396794B CN201310324584.3A CN201310324584A CN103396794B CN 103396794 B CN103396794 B CN 103396794B CN 201310324584 A CN201310324584 A CN 201310324584A CN 103396794 B CN103396794 B CN 103396794B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000843 powder Substances 0.000 title abstract description 24
- PILOURHZNVHRME-UHFFFAOYSA-N [Na].[Ba] Chemical class [Na].[Ba] PILOURHZNVHRME-UHFFFAOYSA-N 0.000 title abstract 2
- 239000000126 substance Substances 0.000 claims abstract description 14
- 229910052788 barium Inorganic materials 0.000 claims abstract description 13
- 230000005284 excitation Effects 0.000 claims abstract description 6
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 5
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 40
- 238000001354 calcination Methods 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 150000001875 compounds Chemical class 0.000 claims description 18
- 230000003213 activating effect Effects 0.000 claims description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 8
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 238000005286 illumination Methods 0.000 claims description 5
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 5
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical compound [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 239000004317 sodium nitrate Substances 0.000 claims description 4
- 229940001516 sodium nitrate Drugs 0.000 claims description 4
- 235000010344 sodium nitrate Nutrition 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000003836 solid-state method Methods 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 description 9
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 8
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 239000003513 alkali Substances 0.000 description 6
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 238000012544 monitoring process Methods 0.000 description 5
- 239000002585 base Substances 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 238000000695 excitation spectrum Methods 0.000 description 4
- 238000000634 powder X-ray diffraction Methods 0.000 description 4
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 4
- 238000013459 approach Methods 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 1
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 208000019048 congenital factor V deficiency Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- -1 europium ion Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000000891 luminescent agent Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 1
- 125000000101 thioether group Chemical group 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 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
Landscapes
- Luminescent Compositions (AREA)
Abstract
The invention discloses Eu<3+> activated sodium barium tungstate fluorescent powder, a preparation method and an application thereof. The chemical formula of the fluorescent powder is M4-xEuxNa2W2O11, wherein M is one of Ba, Sr and Ca, and is more than or equal to 0.001 and less than or equal to 0.3; the fluorescent powder which is obtained by adopting a high temperature solid state method, can emit red fluorescent light with the wavelength of 590-720nm under the excitation of near ultraviolet ray, is good in chemical stability and high in red light intensity, can be matched with near ultraviolet and blue LEDs (light emitting diodes), and is novel red fluorescent powder for white light LEDs. The preparation method is simple, low in production cost and easy for industrial production.
Description
Technical field
The present invention relates to a kind of inorganic fluorescent material, preparation method and application thereof, be specifically related to one under near ultraviolet excitation, launch a kind of tungstate base fluorescent powder of red fluorescence, can apply and be packaged in outside InGaN diode, prepare White-light LED illumination device.
Background technology
The plurality of advantages such as that white light LEDs (Light Emitting Diode) has is nontoxic, energy-efficient, the life-span long, shock resistance and safety are decided.Can be widely used on various lighting installations, be a kind of environmental protection, energy-conservation green illumination light source, caused the attention of many national government and scientific and technological circle and industrial community and formulated development program.
Realize at present White-light LED illumination and mainly contain 3 kinds of approach.The first approach is to be combined to form white light by red, green and blue look LED chip; The second approach is to use quantum effect to realize Single chip white light, and the third is to add that with the chip of sending out UV-light or blue light fluorescent material realizes white light.The third method be cost minimum, simple, be simultaneously also the most ripe method.This kind of fluorescent material is mainly YAG yttrium aluminum garnet at present, and its chemical formula is Y
3al
5o
12: Ce
3+, the white light LEDs that this fluorescent material is made has very high luminous efficiency, but because the few colour rendering index that makes of ruddiness comparison of ingredients in emmission spectrum is on the low side, colour temperature is higher.This has just reduced the application of white light LEDs at low colour temperature, warm white lighting field.LED is mainly Y with business red fluorescence powder at present
2o
2s:Eu
3+, this red fluorescence powder is sulfide, preparation method's complexity, and luminous efficiency is low.The red fluorescence powder that therefore develop a kind of low cost, stable performance, can efficiently be excited by UV-light, purple light or blue-light LED chip has just become at present the focus of research both at home and abroad.
The tungstate red fluorescent powder that Eu excites has various features, tungstate red fluorescent powder has satisfactory stability, sulfide or the labile deficiency of oxysulfide red fluorescence powder are overcome, become gradually the focus of research, over entering year, rear-earth-doped tungstate red fluorescent powder has been subject to paying close attention to widely.
Summary of the invention
The object of the present invention is to provide that a kind of luminous efficiency is high, stable chemical nature, and the simple Eu of preparation method
3+the sodium wolframate barium fluorescent material, preparation method and the application thereof that activate.
The technical scheme that realizes the object of the invention is to provide a kind of Eu
3+the sodium wolframate barium fluorescent material activating, its chemical formula is M
4-xeu
xna
2w
2o
11, wherein, M is the one in Ba, Sr, Ca, 0.001≤
x≤ 0.3; Described fluorescent material, under near ultraviolet excitation, is launched the red fluorescence that wavelength is 590～720 nanometers.
A kind of Eu as above
3+the preparation method of the sodium wolframate barium fluorescent material activating, comprises the steps:
1, to contain the compound of M element, the compound that contains Na element, the compound that contains Eu element, the compound that contains W element is raw material, by chemical formula M
4-xeu
xna
2w
2o
11the stoichiometric ratio of middle corresponding element takes each raw material, and in formula, M is the one in Ba, Sr, Ca, 0.001≤
x≤ 0.3; After grinding respectively, mix;
2, by the raw material mixing presintering in air, sintering temperature is 200～600 DEG C, and sintering time is 2～10 hours;
3, the product obtaining is ground and mixed, in air atmosphere, calcine, calcining temperature is 700～1000 DEG C, and calcination time is 2～18 hours, obtains a kind of Eu
3+the sodium wolframate barium fluorescent material activating.
The compound of the M of containing element of the present invention is the one in the oxide compound that contains M element, carbonate, nitrate.The described compound that contains Na element is the one in sodium hydroxide, sodium carbonate, SODIUMNITRATE.The described compound that contains Eu element is the one in europium sesquioxide, europium nitrate.The described compound that contains W element is the one in Tungsten oxide 99.999, ammonium tungstate.
In preparation method provided by the invention, preferred scheme is: the sintering temperature described in step 2 is 350～600 DEG C, and sintering time is 3～8 hours.Calcining temperature described in step 3 is 750～950 DEG C, and calcination time is 3～15 hours.
Eu provided by the invention
3+the application of the sodium wolframate barium fluorescent material activating is: coordinated appropriate blueness and green emitting phosphor, apply and be packaged in outside diode, for the preparation of White-light LED illumination device.
Compared with prior art, the advantage of technical solution of the present invention is:
1, the present invention is to provide a kind of trivalent europium ion Eu
3+the sodium wolframate barium base fluorescent powder activating, its main emission peak is in 613nm left and right, and it has very strong launching efficiency in the near ultraviolet region of 395nm, and this region is just the radiation wavelength of near ultraviolet LED chip, is therefore a kind of good red fluorescent powder for white radiation LED.
2, can effectively absorb near the exciting of 395nm, its main emission peak, in 613nm left and right, coordinates with green emitting phosphor, is coated on blue-light LED chip and can prepares novel white light LEDs.
3, the Eu that prepared by the present invention
3+the sodium wolframate barium base fluorescent powder activating, compared with other sulfide, halogenide, its base starting material source is abundant, cheap, and preparation technology is simple, without waste water and gas discharge, environmentally friendly.Have good thermostability, color developing, is conducive to realize the high-power LED of preparation.
Brief description of the drawings
Fig. 1 is the prepared Ba of the embodiment of the present invention 1
3.9eu
0.1na
2w
2o
11the X-ray powder diffraction collection of illustrative plates of material sample;
Fig. 2 is the prepared Ba of the embodiment of the present invention 1
3.9eu
0.1na
2w
2o
11the exciting light spectrogram of material sample under monitoring wavelength 613 nanometers;
Fig. 3 is the prepared Ba of the embodiment of the present invention 1
3.9eu
0.1na
2w
2o
11the luminescent spectrum figure of material sample under 396 nano wave lengths excite;
Fig. 4 is the prepared Ba of the embodiment of the present invention 1
3.9eu
0.1na
2w
2o
11material sample is being monitored under exciting light 266nm, the extinction curve collection of illustrative plates of 613nm;
Fig. 5 is the prepared Ba of the embodiment of the present invention 5
3.7eu
0.3na
2w
2o
11the X-ray powder diffraction collection of illustrative plates of material sample;
Fig. 6 is the prepared Ba of the embodiment of the present invention 5
3.7eu
0.3na
2w
2o
11the exciting light spectrogram of material sample under monitoring wavelength 613 nanometers;
Fig. 7 is the prepared Ba of the embodiment of the present invention 5
3.7eu
0.3na
2w
2o
11the luminescent spectrum figure of material sample under 396 nano wave lengths excite.
Embodiment
Below in conjunction with drawings and Examples, technical solution of the present invention is further elaborated.
Embodiment 1:
Preparation Ba
3.9eu
0.1na
2w
2o
11
According to chemical formula Ba
3.9eu
0.1na
2w
2o
11, take respectively: barium carbonate BaCO
3: 3.8482 grams, europium sesquioxide Eu
2o
3: 0.088 gram, sodium hydroxide: NaOH:0.4001 gram, Tungsten oxide 99.999: WO
3: 2.3184 grams, after grinding and mixing, in air atmosphere, carry out presintering in agate mortar, pre-sintering temperature is 500 DEG C, sintering time 7 hours, is cooled to room temperature, takes out sample; After it is fully ground again, be placed in retort furnace, under air atmosphere, calcine, calcining temperature is 950 DEG C, and calcination time is 10 hours, obtains powder shaped wolframic acid alkali red illuminating material.
Referring to accompanying drawing 1, it is the X-ray powder diffraction collection of illustrative plates of preparing sample by the present embodiment technical scheme, and XRD test result shows, prepared Ba
3.9eu
0.1na
2w
2o
11for monophase materials, exist mutually without any other impurity thing, and degree of crystallinity is better.
Referring to accompanying drawing 2, it is the exciting light spectrogram obtaining under the prepared sample 613 nanometer monitorings of the present embodiment; As can be seen from the figure, the emitting red light of this material excite source mainly near ultraviolet 396 nanometers, can mate well the White-light LED chip of near ultraviolet excitation.
Referring to accompanying drawing 3, it is the luminescent spectrum figure that the prepared sample of the present embodiment obtains under 396 nano wave lengths excite; The main luminescence center of this material is at the emitting red light wave band of 613 nanometers.
Referring to accompanying drawing 4, it is that the prepared sample of the present embodiment is under 266 nanometers at monitoring exciting light, the extinction curve collection of illustrative plates of 613 nano luminescents.Luminescent lifetime is 0.36ms.
Embodiment 2:
Preparation Ba
3.88eu
0.12na
2w
2o
11
According to chemical formula Ba
3.88eu
0.12na
2w
2o
11, take respectively: barium carbonate BaCO
3: 3.8286 grams, europium sesquioxide Eu
2o
3: 0.1056 gram, sodium carbonate: Na
2cO
3: 1.06 grams, Tungsten oxide 99.999: WO
3: 2.3184 grams, after grinding and mixing, in air atmosphere, carry out presintering in agate mortar, pre-sintering temperature is 400 DEG C, sintering time 6 hours, is cooled to room temperature, takes out sample; After it is fully ground again, be placed in retort furnace, under air atmosphere, calcine, calcining temperature is 900 DEG C, and calcination time is 12 hours, obtains powder shaped wolframic acid alkali red illuminating material.Its main structure properties, excitation spectrum and luminescent spectrum are similar to embodiment 1.
Embodiment 3:
Preparation Sr
3.95eu
0.05na
2w
2o
11
According to chemical formula Sr
3.95eu
0.05na
2w
2o
11, take respectively: Strontium carbonate powder SrCO
3: 2.9157 grams, europium nitrate Eu (NO
3)
36H
2o:0.0558 gram, SODIUMNITRATE: NaNO
3: 0.8499 gram, ammonium tungstate: (NH
4)
6w
7o
246H
2o:2.696 gram after grinding and mixing, carries out presintering in agate mortar in air atmosphere, and pre-sintering temperature is 350 DEG C, and sintering time 5 hours, is cooled to room temperature, takes out sample; After it is fully ground again, be placed in retort furnace, under air atmosphere, calcine, calcining temperature is 850 DEG C, and calcination time is 13 hours, obtains powder shaped wolframic acid alkali red illuminating material.Its main structure properties, excitation spectrum and luminescent spectrum are similar to embodiment 1.
Embodiment 4:
Preparation Ca
3.8eu
0.2na
2w
2o
11
According to chemical formula Ca
3.8eu
0.2na
2w
2o
11, take respectively: calcium oxide CaO:1.0655 gram, europium nitrate Eu (NO
3)
36H
2o:0.4461 gram, SODIUMNITRATE: NaNO
3: 0.8499 gram, ammonium tungstate: (NH
4)
6w
7o
246H
2o:2.696 gram after grinding and mixing, carries out presintering in agate mortar in air atmosphere, and pre-sintering temperature is 450 DEG C, and sintering time 8 hours, is cooled to room temperature, takes out sample; After it is fully ground again, be placed in retort furnace, under air atmosphere, calcine, calcining temperature is 850 DEG C, and calcination time is 8 hours, obtains powder shaped wolframic acid alkali red illuminating material.Its main structure properties, excitation spectrum and luminescent spectrum are similar to embodiment 1.
Embodiment 5:
Preparation Sr
3.75eu
0.25na
2w
2o
11
According to chemical formula Sr
3.75eu
0.25na
2w
2o
11, take respectively: Strontium carbonate powder SrCO
3: 2.7685 grams, europium sesquioxide Eu
2o
3: 0.213 gram, sodium hydroxide: NaOH:0.4001 gram, ammonium tungstate: (NH
4)
6w
7o
246H
2o:2.696 gram after grinding and mixing, carries out presintering in agate mortar in air atmosphere, and pre-sintering temperature is 600 DEG C, and sintering time 4 hours, is cooled to room temperature, takes out sample; After it is fully ground again, be placed in retort furnace, under air atmosphere, calcine, calcining temperature is 750 DEG C, and calcination time is 15 hours, obtains powder shaped wolframic acid alkali red illuminating material.Its main structure properties, excitation spectrum and luminescent spectrum are similar to embodiment 1.
Embodiment 6:
Preparation Ba
3.7eu
0.3na
2w
2o
11
According to chemical formula Ba
3.7eu
0.3na
2w
2o
11, take respectively: barium carbonate BaCO
3: 3.6509 grams, europium sesquioxide Eu
2o
3: 0.264 gram, sodium carbonate: Na
2cO
3: 1.06 grams, Tungsten oxide 99.999: WO
3: 2.3184 grams, after grinding and mixing, in air atmosphere, carry out presintering in agate mortar, pre-sintering temperature is 400 DEG C, sintering time 6 hours, is cooled to room temperature, takes out sample; After it is fully ground again, be placed in retort furnace, under air atmosphere, calcine, calcining temperature is 900 DEG C, and calcination time is 12 hours, obtains powder shaped wolframic acid alkali red illuminating material.
Referring to accompanying drawing 5, it is the X-ray powder diffraction collection of illustrative plates of preparing sample by the present embodiment technical scheme, and XRD test result shows, prepared Ba
3.7eu
0.3na
2w
2o
11for monophase materials, exist mutually without any other impurity thing, and degree of crystallinity is better.
Referring to accompanying drawing 6, it is the exciting light spectrogram obtaining under the prepared sample 613 nanometer monitorings of the present embodiment; As can be seen from the figure, the emitting red light of this material excite source mainly near ultraviolet 396 nanometers, can mate well the White-light LED chip of near ultraviolet excitation.
Referring to accompanying drawing 7, it is the luminescent spectrum figure that the prepared sample of the present embodiment obtains under 396 nano wave lengths excite.
Claims (9)
1. an Eu
3+the fluorescent material activating, is characterized in that: its chemical formula is M
4-xeu
xna
2w
2o
11, wherein, M is the one in Ba, Sr, Ca, 0.001≤x≤0.3; Described fluorescent material, under near ultraviolet excitation, is launched the red fluorescence that wavelength is 590～720 nanometers.
2. an Eu as claimed in claim 1
3+the preparation method of the fluorescent material activating, is characterized in that comprising the steps:
(1) to contain the compound of M element, the compound that contains Na element, the compound that contains Eu element, the compound that contains W element is raw material, by chemical formula M
4-xeu
xna
2w
2o
11the stoichiometric ratio of middle corresponding element takes each raw material, and in formula, M is the one in Ba, Sr, Ca, 0.001≤x≤0.3; After grinding respectively, mix;
(2) by the raw material mixing presintering in air, sintering temperature is 200～600 DEG C, and sintering time is 2～10 hours;
(3) product obtaining is ground and mixed, in air atmosphere, calcine, calcining temperature is 700～1000 DEG C, and calcination time is 2～18 hours, obtains a kind of Eu
3+the fluorescent material activating.
3. a kind of Eu according to claim 2
3+the preparation method of fluorescent material who activates, is characterized in that: the described compound that contains M element is the one in the oxide compound that contains M element, carbonate, nitrate.
4. a kind of Eu according to claim 2
3+the preparation method of the fluorescent material activating, is characterized in that: the described compound that contains Na element is the one in sodium hydroxide, sodium carbonate, SODIUMNITRATE.
5. a kind of Eu according to claim 2
3+the preparation method of the fluorescent material activating, is characterized in that: the described compound that contains Eu element is the one in europium sesquioxide, europium nitrate.
6. a kind of Eu according to claim 2
3+the preparation method of the fluorescent material activating, is characterized in that: the described compound that contains W element is the one in Tungsten oxide 99.999, ammonium tungstate.
7. a kind of Eu according to claim 2
3+the preparation method of the fluorescent material activating, is characterized in that: the described sintering temperature of step (2) is 350～600 DEG C, and sintering time is 3～8 hours.
8. a kind of Eu according to claim 2
3+the preparation method of the fluorescent material activating, is characterized in that: the described calcining temperature of step (3) is 750～950 DEG C, and calcination time is 3～15 hours.
9. an Eu as claimed in claim 1
3+the application of the fluorescent material activating, is characterized in that: coordinated appropriate blueness and green emitting phosphor, apply and be packaged in outside diode, for the preparation of White-light LED illumination device.
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|---|---|---|---|
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