CN104371717A - Preparation method for enhancing luminescence property of BiPO4:Eu fluorescent powder by shape regulation - Google Patents
Preparation method for enhancing luminescence property of BiPO4:Eu fluorescent powder by shape regulation Download PDFInfo
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- CN104371717A CN104371717A CN201410605868.4A CN201410605868A CN104371717A CN 104371717 A CN104371717 A CN 104371717A CN 201410605868 A CN201410605868 A CN 201410605868A CN 104371717 A CN104371717 A CN 104371717A
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Abstract
The invention discloses a preparation method for enhancing luminescence property of BiPO4:Eu fluorescent powder by shape regulation. By adopting a hydrothermal process, Bi(NO3)3.5H2O and Eu(NO3)3 react with a NH4H2PO4 solution to synthesize the BiPO4:Eu fluorescent powder. The method comprises the following steps: respectively dissolving a bismuth-europium mixture and phosphate in dilute nitric acid and deionized water in a (Bi+Eu):PO4 ratio of 1:(0.5-10), mixing, stirring, regulating the pH value to 0.5-2 to form a precursor, transferring the precursor into a polytetrafluoroethylene-lined reaction kettle, keeping at the hydrothermal reaction temperature of 140-200 DEG C to react to generate a white precipitate, taking out, washing, and drying to obtain the BiPO4:Eu powder. The hydrothermal process is adopted to quickly synthesize the BiPO4:Eu powder in different shapes. The method is simple to operate and short in preparation period. The BiPO4:Eu fluorescent powder has the advantages of regular crystal, uniform crystal grain, high crystallinity and favorable luminescence property.
Description
Technical field
The present invention relates to phosphor preparation field, particularly relate to a kind of pattern that regulates and strengthen BiPO
4: the preparation method of Eu light-emitting phosphor performance.
Technical background
Phosphor occupies very important status in field of light emitting materials, has been widely used in the fields such as display, artificial lighting, laser, opto-electronic device, fluorescent mark.And phosphor take rare earth luminescent material as representative, its advantage is that sharp line spectrum is launched, and receptivity is strong, and quantum yield rate is high, and physico-chemical property is stablized, and thermostability is high.RE phosphate, because high thermostability and the high-compatibility with rare earth ion, occupies critical role, causes the extensive research of scholars in rare earth luminescent material matrix.But owing to obtaining the with high costs of high purity rare earth ion, scholars wish that finding a kind of main group element (Sb, Bi) substitutes rare earth ion, wherein BiPO
4because of Bi ion and and LnPO similar to Ln system ionic radius
4structural similitude causes extensive research.
Existing white light LEDs adopts 460nm blue chip to become white light LEDs with the YAG:Ce phosphor combination of Yellow light-emitting low temperature, but the white light LEDs color developing that this blue-ray LED+YAG:Ce combines is on the low side, maximumly be only about 85, caused by this is mainly too weak by the range of fluorescent material in red light region, therefore people attempt to develop the secondary fluorescence powder that glows to improve the performance of YAG:Ce.At present, people have studied multiple red fluorescence powder, comprising: molybdate, tungstate, aluminate, phosphoric acid salt etc., wherein bismuth phosphate (BiPO
4) structure that has six side's phases, low temperature monoclinic phase and high temperature monoclinic phase three kinds different, inhomogeneity makes it have different physics and chemistry characteristics, can be used for regulating light; And BiPO
4with lanthanide orthophosphate structural similitude, bismuth ion is identical with trivalent rare earth ions valency, and ionic radius and energy level are more or less the same, due to these advantages, and BiPO
4the extensive research of people is caused as a kind of rare earth ion doped matrix.
2008 years, people's reported first such as Guan BiPO of sea urchin shape
4: Ln has good luminescent properties as a kind of rare earth luminescent material.After this, people are to BiPO
4character, application and preparation carried out studying more and more widely.The people such as Han first with glycerine-water for solvent, with NaH
2pO
4for microcosmic salt, adopt solvent structure BiPO
4: Ce, Tb fluorescent material, have studied the transmission ofenergy of Ce ion to Tb ion.[X.M.Han, G.Y.Zhang, X.W.Qi, X.Q.Wang, M.Y.Li, X.D.Sun, W.Chen, Synthesis andluminescence properties of BiPO
4: Ce, Tb nanorods, J.Lumin.152 (2014) 37-39]; The people such as Sun are first with Bi
2o
3, P
2o
5and Eu
2o
3for raw material, adopt Solid phase synthesis BiPO
4: Eu fluorescent material [X.Y.Sun, X.D.Sun, J.He X.G.Li, J.F.Lv, Synthesis and luminescence of BiPO
4: xEu
3+powders by solid state reaction method, Ceram.Int.40 (2014) 7647-7650].
Preparation method of the prior art, complex process, structure and pattern uncontrollable, obtained BiPO4:Eu fluorescent material, luminescent properties can not meet the demand of practical application.
Summary of the invention
For solving deficiency of the prior art, the invention provides a kind of pattern that regulates and strengthening BiPO
4: the preparation method of Eu light-emitting phosphor performance, the BiPO of the different morphologies that the method has obtained
4: Eu crystal, this BiPO
4: Eu crystal morphology is regular, and grain-size is homogeneous, and degree of crystallinity is high, good dispersity.
Above-mentioned purpose of the present invention is realized by following technological line and measure:
A kind of pattern that regulates strengthens BiPO
4: the preparation method of Eu light-emitting phosphor performance, comprises the following steps:
1) by Bi (NO
3)
35H
2o and Eu (NO
3)
3be dissolved in nitric acid, after stirring, obtain solution A, by NH
4h
2pO
4be dissolved in deionized water and obtain solution B; According to (Bi+Eu): PO
4=1:(0.5 ~ 10) mol ratio, mixed solution A and solution B, stir and obtain presoma;
2) pH value regulating presoma is 0.5 ~ 2;
3) presoma after adjust ph being transferred to liner is in the reactor of tetrafluoroethylene, after sealing hydrothermal reaction kettle, adopts hydrothermal method, under temperature is 140 ~ 200 DEG C of conditions, fully react, naturally cool to room temperature after reaction terminates, obtain white precipitate;
4) taken out by the white precipitate generated, washing, obtains BiPO after drying
4: Eu fluorescent material;
As a further improvement on the present invention, Eu (NO
3)
3concentration be 0.2mol/L.
As a further improvement on the present invention, step 1) in Bi accounts for (Bi+Eu) in solution A molecular fraction be 80% ~ 95%.
As a further improvement on the present invention, step 2) in adopt nitric acid and ammoniacal liquor adjust ph.
As a further improvement on the present invention, described nitric acid is dust technology, and concentration is 2mol/L ~ 3mol/L.
As a further improvement on the present invention, step 3) in the presoma packing ratio be packed in reactor after adjust ph be 65% ~ 85%.
As a further improvement on the present invention, step 3) sufficient reaction time is 4 ~ 24h.
As a further improvement on the present invention, step 4) in adopt deionized water and dehydrated alcohol to wash respectively.
As a further improvement on the present invention, step 4) in drying conditions be that temperature is 70 ~ 80 DEG C, the time is 10 ~ 15h.
Relative to prior art, the present invention has the following advantages:
The present invention is with Bi (NO
3)
35H2O, Eu (NO
3)
3and NH
4h
2pO
4for raw material, with water as solvent, do not using the BiPO of the different morphologies obtained under any template and tensio-active agent condition
4: Eu crystal, regular appearance, grain-size is homogeneous, and degree of crystallinity is high, good dispersity.
The present invention adopts water heat transfer, by regulating (Bi+Eu): PO
4mol ratio is come BiPO
4: the structure of Eu fluorescent material, pattern and luminescent properties regulate and control, and have expanded the control measures of fluorescent material structure, pattern and luminescent properties.Synthetic method hydrothermal method of the present invention is green synthesis method, and technique is simple, and easy to operate, preparation cycle is short;
(Bi+Eu): PO in the present invention
4mol ratio can affect BiPO
4: the pattern of Eu crystal, therefore, it is possible to by regulating Bi+Eu:PO
4mol ratio regulate and control BiPO
4: the pattern of Eu crystal, has the advantage of target crystal crystal phase structure and morphology controllable, and the bar-shaped BiPO prepared
4: Eu fluorescent material has good luminescent properties, has expanded the structure of fluorescent material, pattern, luminescent properties control measures.
The invention provides the novel method of regulate shape under a kind of crystalline structure of the same race, for the impact of pattern on luminescence under studying crystalline phase condition of the same race provides a kind of new approaches.
Accompanying drawing explanation
Fig. 1 a is BiPO prepared by embodiment 1
4: the SEM figure of Eu powder;
Fig. 1 b is BiPO prepared by embodiment 2
4: the SEM figure of Eu powder;
Fig. 1 c is BiPO prepared by embodiment 3
4: the SEM figure of Eu powder;
Fig. 1 d is BiPO prepared by embodiment 4
4: the SEM figure of Eu powder;
Fig. 2 is different (Bi+Eu): PO
4the BiPO prepared under molar ratio
4: the XRD figure spectrum of Eu fluorescent material;
Fig. 3 is different (Bi+Eu): PO
4the BiPO prepared under molar ratio
4: the utilizing emitted light spectrogram of Eu fluorescent material.
Wherein, a is (Bi+Eu): PO
4emmission spectrum when mol ratio is 1:2.5; B is (Bi+Eu): PO
4emmission spectrum when mol ratio is 1:1; C is (Bi+Eu): PO
4emmission spectrum when mol ratio is 1:0.5.
Embodiment
Below in conjunction with specific embodiments and the drawings, the present invention is described in further detail.
Embodiment 1:
Step 1: by 3.8mmol Bi (NO
3)
35H
2o and 1mL concentration is the Eu (NO of 0.2mol/L
3)
3be dissolved in the dust technology of 10mL, stir 30min to evenly, obtain solution liquid A; By 2mmol NH
4h
2pO
4be dissolved in 20mL deionized water, stir 30min to evenly, obtain the solution B that concentration is 0.1mol/L; According to (Bi+Eu): PO
4mol ratio is that solution B dropwise joins in solution A by 1:0.5, obtains precursor liquid, stirs 30min to even;
Step 2: use NH
3h
20 and dust technology regulate the pH value of precursor liquid to be 0.8;
Step 3: precursor liquid being transferred to liner is in the reactor of tetrafluoroethylene, the packing ratio of hydrothermal reaction kettle is 75%, sealing hydrothermal reaction kettle;
Step 4: hydrothermal reaction kettle is put into baking oven, with time of 30min from room temperature to 160 DEG C, then is incubated 16h, then naturally cools to room temperature under 160 DEG C of conditions;
Step 5: the precipitation generated in hydrothermal reaction kettle taken out, wash 3 times respectively with deionized water and dehydrated alcohol, dry 12h, obtains BiPO at 80 DEG C
4: Eu powder.
Fig. 1 a is BiPO prepared by embodiment 1
4: the SEM figure of Eu powder, the BiPO as can be seen from the figure prepared
4: Eu fluorescent material is cocoon-like nano particle.
Embodiment 2:
Step 1: by 3.8mmol Bi (NO
3)
35H
2o and 1mL concentration is the Eu (NO of 0.2mol/L
3)
3be dissolved in the dust technology of 10mL, stir 30min to evenly, obtain solution liquid A; By 4mmol NH
4h
2pO
4be dissolved in 20mL deionized water, stir 30min to evenly, obtain the solution B that concentration is 0.2mol/L; According to (Bi+Eu): PO
4mol ratio is that solution B dropwise joins in solution A by 1:1, obtains precursor liquid, stirs 30min to even;
Step 2: use NH
3h
20 and dust technology regulate the pH value of precursor liquid to be 0.8;
Step 3: precursor liquid being transferred to liner is in the reactor of tetrafluoroethylene, the packing ratio of hydrothermal reaction kettle is 75%, sealing hydrothermal reaction kettle;
Step 4: hydrothermal reaction kettle is put into baking oven, with time of 30min from room temperature to 160 DEG C, then is incubated 16h, then naturally cools to room temperature under 160 DEG C of conditions;
Step 5: the precipitation generated in hydrothermal reaction kettle taken out, wash 3 times respectively with deionized water and dehydrated alcohol, dry 12h, obtains BiPO at 80 DEG C
4: Eu powder.
Fig. 1 b is BiPO prepared by embodiment 2
4: the SEM figure of Eu powder, the BiPO as can be seen from the figure prepared
4: Eu is that octahedra micron is brilliant.
Embodiment 3:
Step 1: by 3.8mmol Bi (NO
3)
35H
2o and 1mL concentration is the Eu (NO of 0.2mol/L
3)
3be dissolved in the dust technology of 10mL, stir 30min to evenly, obtain solution liquid A; By 10mmol NH
4h
2pO
4be dissolved in 20mL deionized water, stir 30min to evenly, obtain the solution B that concentration is 0.5mol/L; According to (Bi+Eu): PO
4mol ratio is that solution B dropwise joins in solution A by 1:2.5, obtains precursor liquid, stirs 30min to even;
Step 2: use NH
3h
20 and dust technology regulate the pH value of precursor liquid to be 0.8;
Step 3: precursor liquid being transferred to liner is in the reactor of tetrafluoroethylene, the packing ratio of hydrothermal reaction kettle is 75%, sealing hydrothermal reaction kettle;
Step 4: hydrothermal reaction kettle is put into baking oven, with time of 30min from room temperature to 160 DEG C, then is incubated 16h, then naturally cools to room temperature under 160 DEG C of conditions;
Step 5: the precipitation generated in hydrothermal reaction kettle taken out, wash 3 times respectively with deionized water and dehydrated alcohol, dry 12h, obtains BiPO at 80 DEG C
4: Eu powder.
Fig. 1 c is BiPO prepared by embodiment 3
4: the SEM figure of Eu powder, the BiPO as can be seen from the figure prepared
4: Eu is micron bar.
Embodiment 4:
Step 1: by 3.8mmol Bi (NO
3)
35H
2o and 1mL concentration is the Eu (NO of 0.2mol/L
3)
3be dissolved in the dust technology of 10mL, stir 30min to evenly, obtain solution liquid A; By 20mmol NH
4h
2pO
4be dissolved in 20mL deionized water, stir 30min to evenly, obtain the solution B that concentration is 1mol/L; According to (Bi+Eu): PO
4mol ratio is that solution B dropwise joins in solution A by 1:5, obtains precursor liquid, stirs 30min to even;
Step 2: use NH
3h
20 and dust technology regulate the pH value of precursor liquid to be 0.8;
Step 3: precursor liquid being transferred to liner is in the reactor of tetrafluoroethylene, the packing ratio of hydrothermal reaction kettle is 75%, sealing hydrothermal reaction kettle;
Step 4: hydrothermal reaction kettle is put into baking oven, with time of 30min from room temperature to 160 DEG C, then is incubated 16h, then naturally cools to room temperature under 160 DEG C of conditions;
Step 5: the precipitation generated in hydrothermal reaction kettle taken out, wash 3 times respectively with deionized water and dehydrated alcohol, dry 12h, obtains BiPO at 80 DEG C
4: Eu powder.
Fig. 1 d is BiPO prepared by embodiment 4
4: the SEM figure of Eu powder, the BiPO as can be seen from the figure prepared
4: Eu fluorescent material is micron bar.
Embodiment 5:
Step 1: by 3.4mmol Bi (NO
3)
35H
2o and 3mL concentration is the Eu (NO of 0.2mol/L
3)
3be dissolved in the dust technology of 10mL 2mol/L, stir 30min to evenly, obtain solution liquid A; By 40mmolNH
4h
2pO
4be dissolved in 20mL deionized water, stir 30min to evenly, obtain the solution B that concentration is 2mol/L; According to (Bi+Eu): PO
4mol ratio is that solution B dropwise joins in solution A by 1:10, obtains precursor liquid, stirs 30min to even;
Step 2: use NH
3h
20 and dust technology regulate the pH value of precursor liquid to be 0.8;
Step 3: precursor liquid being transferred to liner is in the reactor of tetrafluoroethylene, the packing ratio of hydrothermal reaction kettle is 75%, sealing hydrothermal reaction kettle;
Step 4: hydrothermal reaction kettle is put into baking oven, with time of 30min from room temperature to 160 DEG C, then is incubated 16h, then naturally cools to room temperature under 160 DEG C of conditions;
Step 5: the precipitation generated in hydrothermal reaction kettle taken out, wash 3 times respectively with deionized water and dehydrated alcohol, dry 12h, obtains BiPO at 80 DEG C
4: Eu powder.
Embodiment 6:
Step 1: by 3.2mmol Bi (NO
3)
35H
2o and 4mL concentration is the Eu (NO of 0.2mol/L
3)
3be dissolved in the dust technology of 10mL, stir 30min to evenly, obtain solution liquid A; By 2mmol NH
4h
2pO
4be dissolved in 20mL deionized water, stir 30min to evenly, obtain the solution B that concentration is 0.1mol/L; According to (Bi+Eu): PO
4mol ratio is that solution B dropwise joins in solution A by 1:0.5, obtains precursor liquid, stirs 30min to even;
Step 2: use NH
3h
20 and dust technology regulate the pH value of precursor liquid to be 0.5;
Step 3: precursor liquid being transferred to liner is in the reactor of tetrafluoroethylene, the packing ratio of hydrothermal reaction kettle is 65% ~ 85%, sealing hydrothermal reaction kettle;
Step 4: hydrothermal reaction kettle is put into baking oven, with time of 30min from room temperature to 140 DEG C, then is incubated 24h, then naturally cools to room temperature under 140 DEG C of conditions;
Step 5: the precipitation generated in hydrothermal reaction kettle taken out, wash 3 times respectively with deionized water and dehydrated alcohol, dry 10h, obtains BiPO at 70 DEG C
4: Eu powder.
Embodiment 7:
Step 1: by 3.6mmol Bi (NO
3)
35H
2o and 2mL concentration is the Eu (NO of 0.2mol/L
3)
3be dissolved in the dust technology of 10mL, stir 30min to evenly, obtain solution liquid A; By 32mmol NH
4h
2pO
4be dissolved in 20mL deionized water, stir 30min to evenly, obtain the solution B that concentration is 1.6mol/L; According to (Bi+Eu): PO
4mol ratio is that solution B dropwise joins in solution A by 1:8, obtains precursor liquid, stirs 30min to even;
Step 2: use NH
3h
20 and dust technology regulate the pH value of precursor liquid to be 2;
Step 3: precursor liquid being transferred to liner is in the reactor of tetrafluoroethylene, the packing ratio of hydrothermal reaction kettle is 65% ~ 85%, sealing hydrothermal reaction kettle;
Step 4: hydrothermal reaction kettle is put into baking oven, with time of 30min from room temperature to 200 DEG C, then is incubated 4h, then naturally cools to room temperature under 200 DEG C of conditions;
Step 5: the precipitation that generates in hydrothermal reaction kettle taken out, wash 3 times respectively with deionized water and dehydrated alcohol, the white precipitate taking-up that will generate after react, with deionized water and absolute ethanol washing 3 times, at 75 DEG C, dry 15h, obtains BiPO
4: Eu powder.
Test result below in conjunction with corresponding embodiment is further analyzed the performance that the present invention obtains product.
Fig. 2 is that the present invention is at different (Bi+Eu): PO
4the BiPO prepared under molar ratio
4: the XRD figure of Eu crystal, wherein a is (Bi+Eu) that embodiment 1 obtains: PO
4mol ratio mol ratio is the BiPO of 1:0.5
4: the XRD figure of Eu crystal; B is (Bi+Eu) that embodiment 2 obtains: PO
4mol ratio is the BiPO of 1:1
4: the XRD figure of Eu crystal, c is (Bi+Eu) that embodiment 3 obtains: PO
4mol ratio is the BiPO of 1:2.5
4: the XRD figure of Eu crystal.As can be seen from Figure 2, as (Bi+Eu): PO
4when mol ratio is 1:0.5, the diffraction peak of the BiPO4:Eu crystal of preparation is all consistent with PDF card (JCPDS NO.15-0766), is six side's phases; As (Bi+Eu): PO
4when mol ratio is 1:1,1:2.5, the BiPO of preparation
4: the diffraction peak of Eu crystal is consistent with PDF card (JCPDS NO.15-0767), is low temperature monoclinic phase.Although b, c are same crystalline phase, by comparing b, the diffraction peak intensity of c, we can find out that the Solute Content in Grain of these two samples is different, this and Fig. 1 b, the result of 1c reflection is consistent, for we study crystalline structure of the same race under the impact of pattern on luminescence a kind of new approaches are provided.
Fig. 3 is difference of the present invention (Bi+Eu): PO
4the BiPO prepared under molar ratio
4: Eu crystal is at near-ultraviolet light (λ
ex=395nm) excite under emmission spectrum, wherein a is (Bi+Eu): PO
4emmission spectrum when mol ratio is 1:2.5; B is (Bi+Eu): PO
4emmission spectrum when mol ratio is 1:1; C is (Bi+Eu): PO
4emmission spectrum when mol ratio is 1:0.5.As can be seen from Figure 3 as (Bi+Eu): PO
4when mol ratio is 1:0.5, emmission spectrum is extremely low, but the characteristic spectrum of Eu still exists, as shown in inset of fig. 3; BiPO
4: the emissive porwer of Eu fluorescent material is along with (Bi+Eu): PO
4the increase of mol ratio strengthens.
The foregoing is only one embodiment of the present invention, it not whole or unique embodiment, the conversion of those of ordinary skill in the art by reading specification sheets of the present invention to any equivalence that technical solution of the present invention is taked, is claim of the present invention and contains.
Claims (9)
1. one kind regulates pattern to strengthen BiPO
4: the preparation method of Eu light-emitting phosphor performance, is characterized in that, comprise the following steps:
1) by Bi (NO
3)
35H
2o and Eu (NO
3)
3be dissolved in nitric acid, after stirring, obtain solution A, by NH
4h
2pO
4be dissolved in deionized water and obtain solution B; According to (Bi+Eu): PO
4=1:(0.5 ~ 10) mol ratio, mixed solution A and solution B, stir and obtain presoma;
2) pH value regulating presoma is 0.5 ~ 2;
3) presoma after adjust ph being transferred to liner is in the reactor of tetrafluoroethylene, after sealing hydrothermal reaction kettle, adopts hydrothermal method, under temperature is 140 ~ 200 DEG C of conditions, fully react, naturally cool to room temperature after reaction terminates, obtain white precipitate;
4) taken out by the white precipitate generated, washing, obtains BiPO after drying
4: Eu fluorescent material.
2. one according to claim 1 regulates pattern to strengthen BiPO
4: the preparation method of Eu light-emitting phosphor performance, is characterized in that: Eu (NO
3)
3concentration be 0.2mol/L.
3. one according to claim 1 regulates pattern to strengthen BiPO
4: the preparation method of Eu light-emitting phosphor performance, is characterized in that: step 1) in Bi accounts for (Bi+Eu) in solution A molecular fraction be 80% ~ 95%.
4. one according to claim 1 regulates pattern to strengthen BiPO
4: the preparation method of Eu light-emitting phosphor performance, is characterized in that: step 2) in adopt nitric acid and ammoniacal liquor adjust ph.
5. the one according to claim 1 or 3 regulates pattern to strengthen BiPO
4: the preparation method of Eu light-emitting phosphor performance, is characterized in that: described nitric acid is dust technology, and concentration is 2mol/L ~ 3mol/L.
6. one according to claim 1 regulates pattern to strengthen BiPO
4: the preparation method of Eu light-emitting phosphor performance, is characterized in that: step 3) in the presoma packing ratio be packed in reactor after adjust ph be 65% ~ 85%.
7. one according to claim 1 regulates pattern to strengthen BiPO
4: the preparation method of Eu light-emitting phosphor performance, is characterized in that: step 3) sufficient reaction time is 4 ~ 24h.
8. one according to claim 1 regulates pattern to strengthen BiPO
4: the preparation method of Eu light-emitting phosphor performance, is characterized in that: step 4) in adopt deionized water and dehydrated alcohol to wash respectively.
9. one according to claim 1 regulates pattern to strengthen BiPO
4: the preparation method of Eu light-emitting phosphor performance, is characterized in that: step 4) in drying conditions be that temperature is 70 ~ 80 DEG C, the time is 10 ~ 15h.
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