CN106635003A - Lithium ion doped bismuth phosphate samarium fluorescent powder and preparation method thereof - Google Patents
Lithium ion doped bismuth phosphate samarium fluorescent powder and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a lithium ion doped bismuth phosphate samarium fluorescent powder and a preparation method thereof. The preparation method comprises the following steps: firstly, mixing solid powder of Bi(NO3)3*5H2O, Sm(NO3)3*6H2O and LiNO3, adding into a nitric acid solution, uniformly stirring to react to generate Bi0.95NO3:0.05Sm<3+> and Li<+>, further dropping a NH4H2PO4 solution into the solution, continuously stirring until the NH4H2PO4 solution is sufficiently dissolved, adjusting the pH value of a mixed solution B to be 0.50-0.55, performing reaction on the mixed solution at a temperature of 180-185 DEG C to generate precipitate, when the precipitate is not increased, naturally cooling to the room temperature, performing centrifugal separation on the obtained precipitate, washing and drying, and finally obtaining the lithium ion doped bismuth phosphate samarium fluorescent powder. The structure and the lighting property of a product can be affected by adjusting the addition amount of LiNO3, and the prepared fluorescent powder is high in crystallization degree and high in lighting intensity.
Description
【Technical field】
The present invention relates to rare earth luminescent material field, with being related to a kind of lithium ion doped bismuth phosphate samarium fluorescent material and its system
Preparation Method.
【Background technology】
Rare earth luminescent material occupies critically important status in whole solid luminescence field, because special electron structure makes
Rare earth element has the incomparable property of general element.In recent years, because having, absorbability was strong, luminosity is high, conjunction
The advantages of into moderate temperature, RE phosphate is wide in illumination, quantum optices, colour television set and thermoluminescence detection field application
It is general, cause the extensive interest of researcher.Therefore, find that manufacture craft is simple and product multifunction and special appearance
RE phosphate method either in industrial production or scientific research all have important value, also synthesize other receive
Rice material aspect has directive significance.
BiPO4It is a kind of important inorganic phosphate salt material, with three kinds of hexagonal phase, low temperature monoclinic phase and high temperature monoclinic phase
Different structures, be widely used in photocatalysis, ion transducer, lithium ion battery, radioactive element separation, micro-wave dielectric,
The aspects such as ultracapacitor.The performance of the material depends greatly on its pattern, size, structure and its composition.Close
In BiPO4:Ln3+The research of fluorescent material has been achieved with great success, existing solid phase method, microwave-hydrothermal method, solvent-thermal method, co-precipitation
Various methods such as method, method of electrostatic spinning, phonochemistry method, hydro-thermal method are prepared for the BiPO of various structures pattern4:Ln3+Crystal.It is above-mentioned
In synthetic method, hydro-thermal method process is simple, reaction condition is gentle, can well control the pattern of product, size, structure, with this
Simultaneously surfactant also plays important role in control crystal morphology in structure.2008, Guan et al. reported firsts
The sea urchin shape microballoon BiPO that is made up of nanometer rods4:Ln3+(Eu3+, Tb3+, Dy3+) fluorescent material has excellent luminescent properties, it is
A kind of excellent rare earth luminescent material matrix, have studied different Bi3+The impact of ion concentration and reaction time to pattern, it is proposed that
Sea urchin shape microballoon synthesis mechanism (Crystal Growth and Design, 2008,8 (8):2694-2697.)；Shi Xiaolei etc.
People synthesizes BiPO by hydro-thermal method4:Sm3+Orange red fluorescent powder, and have studied different pH value and Sm3+Doping is to its luminescent material
Structure, pattern and luminescent properties impact.(Ceramics International, 2015,41：3162–3168).
The method that Joanna Cybinska et al. are synthesized first using the microwave of ionic liquid auxiliary, have studied BiPO4:Ln3+(Ln=
Sm, Eu, Tb, Dy) rare earth ion doped Color tunable control luminescent material (Journal of Luminescence, 2016,
170:641-647)。
So far, BiPO obtained in existing synthetic method4:Sm3+Fluorescent material degree of crystallinity is low, luminous intensity is not high, also
Nobody proposes that its luminous simple and convenient method can be strengthened.
【The content of the invention】
It is an object of the invention to overcome defect present in prior art, there is provided a kind of lithium ion doped bismuth phosphate samarium is glimmering
Light powder and preparation method thereof, the method technological process is simple, and cost is relatively low, and obtained fluorescent material has degree of crystallinity high, lights strong
The high advantage of degree.
In order to achieve the above object, the inventive method is adopted the following technical scheme that：
Comprise the following steps：
(1) Bi (NO are taken3)3·5H2O、Sm(NO3)3·6H2O and LiNO3Salpeter solution is added to after pressed powder mixing
In, it is uniformly mixing to obtain mixed solution A；
(2) in mixed solution A NH is added dropwise again4H2PO4Solution, continues to stir until NH4H2PO4Solution fully dissolves, and obtains
To mixed solution B；Wherein Bi (NO3)3·5H2O、Sm(NO3)3·6H2O、LiNO3And NH4H2PO4Ratio be 3.8mmol：
0.2mmol：xmmol：4mmol, x=0.1～1.0；
(3) pH value of mixed solution B is adjusted to 0.50～0.55, obtain mixed solution C；
(4) mixed solution C reacts generation precipitation at 180 DEG C～185 DEG C, when not increasing to precipitation, naturally cools to room
Temperature；
(5) the sediment centrifugation for obtaining step (4), the sediment being centrifugally separating to obtain is washed and is dried, and is obtained
To lithium ion doped bismuth phosphate samarium fluorescent material.
Further, the volume fraction of salpeter solution is 13%～13.6% in step (1)；NH in step (2)4H2PO4It is molten
Liquid is by NH4H2PO4Add and stir in deionized water obtained in 20～30min, its concentration is 0.2～0.4mol/L；Salpeter solution
And NH4H2PO4Ratio be 10mL：4mmol.
Further, 10～15min of stirring obtains mixed solution A in step (1).
Further, 20～30min of stirring obtains mixed solution B in step (2).
Further, in step (4), mixed solution C first stirs 40～60min, is then transferred to band polytetrafluoroethyllining lining
Stainless steel cauldron in sealing reaction.
Further, stainless steel cauldron volume compactedness is 80%.
Further, 12～13h of reaction in step (4).
Further, in step (5) centrifugation be rotating speed be 10000r/min under conditions of centrifugation 5～
6min；Washing is to be washed twice with water, and then be washed once with ethanol.
Further, the drying in step (5) is that 10～12h is dried in 75～85 DEG C of drying boxes.
One kind utilizes lithium ion doped bismuth phosphate samarium fluorescent material obtained in method prepared as described above, it is characterised in that：Should
Lithium ion doped bismuth phosphate samarium fluorescent material is monocline phase structure, and size is between 0.5～3 μm.
Compared with prior art, the present invention has following beneficial technique effect：
In preparation method of the present invention, with advantages below：(1) present invention is with Bi (NO3)3·5H2O、Sm(NO3)3·6H2O
And LiNO3And NH4H2PO4Deng for raw material, the BiPO synthesized using hydro-thermal method4:Sm3+Fluorescent material, technological process is simple, cost compared with
It is low, by adjusting LiNO3Addition can just control the luminous intensity of product, be adapted to batch production.(2) present invention is by adding
Plus LiNO3Hydrothermal Synthesiss BiPO4:Sm3+Fluorescent material, as a result proves, adds LiNO3BiPO can more be improved4:Sm3+Fluorescent material it is luminous
Performance.Li is added by hydro-thermal method+Synthesis BiPO4:Sm3+Fluorescent material degree of crystallinity is high, and luminous intensity is high.And also not over hydro-thermal
Method prepares addition Li+BiPO can be improved4:Sm3+The relevant report of light-emitting phosphor performance.(4) present invention adds Li by hydro-thermal method+
Synthesis BiPO4:Sm3+Fluorescent material, its luminescent properties are obviously improved significant to studying luminescent material.
Obtained Li of the invention+Doping BiPO4:Sm3+Fluorescent material be monocline phase structure, size between 0.5～3 μm, phase
BiPO to not adding Li4:Sm3+Fluorescent material, light-emitting phosphor intensity of the present invention improves 1.07～1.5 times, to developing BiPO4
Base fluorescent material is significant.
【Description of the drawings】
Fig. 1 is the present invention by different Li+Addition Hydrothermal Synthesiss Bi0.95PO4:0.05Sm3+The XRD of fluorescent material；
Fig. 2 is the present invention by different Li+Addition Hydrothermal Synthesiss Bi0.95PO4:0.05Sm3+The luminous collection of illustrative plates of fluorescent material.
【Specific embodiment】
Below in conjunction with the accompanying drawings, the present invention is described in further detail.
The present invention is with Bi (NO3)3·5H2O、Sm(NO3)3·6H2O and LiNO3And NH4H2PO4Deng for raw material, by hydro-thermal
Method has synthesized the BiPO of more high luminous intensity4:Sm3+Fluorescent material, have studied different Li+Addition is to BiPO4:Sm3+Structure and send out
The impact of optical property.
Preparation method of the present invention, comprises the following steps：
(1)Bi(NO3)3·5H2O、Sm(NO3)3·6H2O, 0～1.0mmol LiNO3With 0.2～0.4mol/L's
NH4H2PO4Solution, it is standby；Wherein NH4H2PO4Solution is by NH4H2PO4In adding deionized water, 20～30min of stirring makes its molten
Solution, it is standby；
(2) step 1 is taken) standby Bi (NO3)3·5H2O、Sm(NO3)3·6H2O and 0～1.0mmol LiNO3Mixing, will
It is dissolved in the salpeter solution that volume fraction is 13%～13.6%, with 10～15min of stirring to uniformly obtaining mixed solution A,
That is reaction generates Bi0.95NO3：0.05Sm3+,Li+, then NH is added dropwise in mixed solution A4H2PO4Solution, continuation stirring 20～
30min fully dissolves until reagent, obtains mixed solution B；Wherein Bi (NO3)3·5H2O、Sm(NO3)3·6H2O、LiNO3, nitre
Acid solution and NH4H2PO4Ratio be 3.8mmol：0.2mmol：xmmol：10mL：4mmol, x=0.1～1.0；
(3) regulating step 2) pH value of mixed solution B that obtains, to 0.50～0.55, obtains mixed solution C；
(4) by step 3) mixed solution C stir 40～60min after, be transferred to band teflon-lined stainless steel
Seal in reactor, and reactor volume compactedness is 80%, and 12～13h is reacted at 180 DEG C～185 DEG C to generating precipitation,
To precipitation do not increase when, after naturally cool to room temperature；
(5) by step 4) sediment that obtains 5～6min of centrifugation under conditions of rotating speed is 10000r/min, after will
Sediment after centrifugation, is washed twice with water, and is then washed with ethanol 1 time, after be put in 75～85 DEG C of drying boxes be dried 10
～12h, finally prepares addition Li by hydro-thermal method+Strengthen BiPO4:Sm3+The fluorescent material of luminescent properties.
The present invention prepares addition Li by hydro-thermal method+Strengthen BiPO4:Sm3+The fluorescent material of luminescent properties, sample crystallinity is good
It is good, belong to pure cryogenic monoclinic phase, its luminescent properties is significantly increased.
The present invention is described in further details with reference to specific embodiment.
Comparative example 1：
(1) 3.8mmol (1.843g) Bi (NO are taken3)3·5H2O and 0.2mmol (0.089g) Sm (NO3)3·6H2O is put into burning
Cup mixing, then be dissolved in the 10mL salpeter solutions that volume fraction is 13%, magnetic agitation 15min obtains mixed solution A；
(2) 4mmolNH is weighed4H2PO4In being dissolved in 20mL deionized waters, stirring 30min is configured to 0.2mol/L's
NH4H2PO4Solution, is added dropwise in the mixed solution A obtained by step (1), stirs 30min, it is ensured that it is well mixed, and obtains
Mixed solution B；Wherein Bi (NO3)3、Sm(NO3)3·6H2O, salpeter solution and NH4H2PO4Ratio be 3.8mmol：0.2mmol：
10mL：4mmol.
(3) mixed solution C is obtained with the pH=0.5 of dust technology regulation mixed solution B under agitation；
(4) above-mentioned mixed solution C is stirred into 60min, it is close in being transferred to band teflon-lined stainless steel cauldron
Envelope, after reacting 12h at 180 DEG C, naturally cools to room temperature；
(5) by the sediment centrifugation for obtaining (rotating speed is 10000r/min), centrifugation time is 5min, and with water and second
Alcohol repeated washing sediment, centrifugation is put in 80 DEG C of drying boxes after washing and is dried 11h, obtains hydro-thermal method synthesis
Bi0.95PO4:0.05Sm3+Fluorescent material.
Embodiment 1
(1) 3.8mmol (1.843g) Bi (NO are taken3)3·5H2O、0.2mmol(0.089g)Sm(NO3)3·6H2O and
0.1mmol(0.007g)LiNO3Beaker mixing is put into, then is dissolved in the 10mL salpeter solutions that volume fraction is 13%, magnetic
Power stirs 15min, obtains mixed solution A；
(2) 4mmolNH is weighed4H2PO4In being dissolved in 20mL deionized waters, stirring 30min is configured to 0.2mol/L's
NH4H2PO4Solution, is added dropwise in the mixed solution A obtained by step (1), stirs 30min, it is ensured that it is well mixed, and obtains
Mixed solution B；Wherein Bi (NO3)3、Sm(NO3)3·6H2O、LiNO3, salpeter solution and NH4H2PO4Ratio be 3.8mmol：
0.2mmol：0.1mmol：10mL：4mmol.
(3) mixed solution C is obtained with the pH=0.5 of dust technology regulation mixed solution B under agitation；
(4) above-mentioned mixed solution C is stirred into 60min, it is close in being transferred to band teflon-lined stainless steel cauldron
Envelope, after reacting 12h at 180 DEG C, naturally cools to room temperature；
(5) by the sediment centrifugation for obtaining (rotating speed is 10000r/min), centrifugation time is 5min, and with water and second
Alcohol repeated washing sediment, centrifugation is put in 80 DEG C of drying boxes after washing and is dried 11h, obtains the addition of hydro-thermal method synthesis
Li+Strengthen BiPO4:Sm3+The fluorescent material of luminescent properties.
The present embodiment is by changing LiNO3Addition, to study LiNO3Impact to pattern and its luminescent properties.
By the LiNO that the amount of material is 0.1mmol (0.007g)3It is 0.2mmol that powder is substituted for the amount of material
(0.014g), 0.4mmol (0.028g), 0.6mmol (0.041g), the LiNO of 1.0mmol (0.069g)3Powder, and add respectively
Enter to Bi (NO3)3·5H2O and Sm (NO3)3·6H2In the beaker of O hybrid solid powder；Other conditions are same as Example 1.Knot
Comparative example 1 is closed, now LiNO3With Sm (NO3)3·6H2The ratio of O is respectively 0,0.5,1,2,3 and 5.
Fig. 1 is different Li+Addition Hydrothermal Synthesiss Bi0.95PO4:0.05Sm3+The XRD of fluorescent material.Can from figure
Go out, in Li+Addition and Sm3+Ratio when being 0～5, the diffraction maximum of sample and PDF standard cards (space group P21/n (14),
JCPDS15-0767) it coincide, occurs without other diffraction maximums, each sample structure is low temperature monoclinic phase, and degree of crystallinity is higher.With
Li+Addition and Sm3+Ratio increase to during 5 from 0, degree of crystallinity reduces by a small margin.From crystal face (011), (- 111),
(120), (012) is it can be seen that peak height has declined, it follows that, appropriate Li+Addition to Bi0.95PO4:0.05Sm3+Fluorescent material
Structure have some to act on, but have no effect on the essential structure of its pure low temperature monoclinic phase.Above analysis shows, need addition suitable
The LiNO of amount3, pure cryogenic monoclinic phase (low temperature monoclinic phase is conducive to improving luminescent properties) can be just obtained, luminous intensity is reached most
It is high.
Fig. 2 is different Li+Addition Hydrothermal Synthesiss Bi0.95PO4:0.05Sm3+Launching light of the fluorescent material in the case where 402nm is excited
Spectrogram.As seen from the figure, different Li+Addition does not change the transmitting peak shape and peak position of emission spectrum, only intensity of emission spectra with
Li+There is change in addition.Relative to 0.2mmolSm (NO3)3·6H2For O, work as LiNO3Addition is in 0-0.6mmol scopes
It is interior, with LiNO3The increase of addition, the intensity of emission spectra of fluorescent material gradually strengthens, in LiNO3Addition is for 0.6mmol
Sm(NO3)3·6H2O：LiNO3=1:Luminescent properties reach most preferably when 3, work as LiNO3After addition is more than 0.6mmol, emission spectrum
Intensity is slightly reduced, but relative to without LiNO3When luminous intensity still significantly increase.Work as LiNO3Addition exists
In the range of 0-0.6mmol, its lifting of addition to luminescent properties has facilitation, in LiNO3When addition is 1.0mmol, by
The Li in sample+Excessively, Bi can be affected0.95PO4:0.05Sm3+, there is the phenomenon that degree of crystallinity slightly declines in the structure of fluorescent material, can
Li can be because+The Lacking oxygen substantial increase for occupying, makes lattice dilation so as to the degree of crystallinity for causing sample declines, therefore launching light
Spectral intensity has also declined.
It follows that LiNO3Addition is to Bi0.95PO4:0.05Eu3+Light-emitting phosphor performance has a major impact, and it is tied
Structure and pattern also have a certain impact.Work as LiNO3When addition is in the range of 0-1.0mmol, sample structure remains pure cryogenic
Monoclinic phase, with LiNO3Addition increases, and the intensity of emission spectra of fluorescent material gradually strengthens, in LiNO3Addition is 0.6mmol
That is Sm (NO3)3·6H2O：LiNO3=1:Luminescent properties reach most preferably when 3, work as LiNO3After addition is more than 0.6mmol, launching light
Spectral intensity is slightly reduced, but relative to without LiNO3When luminous intensity still significantly increase, be relatively free of addition
Li's, its luminous intensity at least brings up to original 1.07 times, and highest brings up to original 1.5 times.
Embodiment 2：
(1) 3.8mmol (1.843g) Bi (NO are taken3)3·5H2O、0.2mmol(0.089g)Sm(NO3)3·6H2O and
0.2mmol(0.014g)LiNO3Beaker mixing is put into, then is dissolved in the 10mL salpeter solutions that volume fraction is 13%, magnetic
Power stirs 15min, obtains mixed solution A；
(2) 4mmolNH is weighed4H2PO4In being dissolved in 20mL deionized waters, stirring 25min is configured to 0.2mol/L's
NH4H2PO4Solution, is added dropwise in the mixed solution A obtained by step (1), stirs 30min, it is ensured that it is well mixed, and obtains
Mixed solution B；Wherein Bi (NO3)3、Sm(NO3)3·6H2O、LiNO3, salpeter solution and NH4H2PO4Ratio be 3.8mmol：
0.2mmol：0.2mmol：10mL：4mmol.
(3) mixed solution C is obtained with the pH=0.51 of dust technology regulation mixed solution B under agitation；
(4) above-mentioned mixed solution C is stirred into 60min, it is close in being transferred to band teflon-lined stainless steel cauldron
Envelope, after reacting 12h at 182 DEG C, naturally cools to room temperature；
(5) by the sediment centrifugation for obtaining (rotating speed is 10000r/min), centrifugation time is 5min, and with water and second
Alcohol repeated washing sediment, centrifugation is put in 80 DEG C of drying boxes after washing and is dried 12h, obtains the addition of hydro-thermal method synthesis
Li+Strengthen BiPO4:Sm3+The fluorescent material of luminescent properties.
Embodiment 3：
(1) 3.8mmol (1.843g) Bi (NO are taken3)3·5H2O、0.2mmol(0.089g)Sm(NO3)3·6H2O and
0.4mmol(0.028g)LiNO3Beaker mixing is put into, then is dissolved in the 10mL salpeter solutions that volume fraction is 13%, magnetic
Power stirs 15min, obtains mixed solution A；
(2) 4mmolNH is weighed4H2PO4In being dissolved in 20mL deionized waters, stirring 20min is configured to 0.2mol/L's
NH4H2PO4Solution, is added dropwise in the mixed solution A obtained by step (1), stirs 30min, it is ensured that it is well mixed, and obtains
Mixed solution B；Wherein Bi (NO3)3、Sm(NO3)3·6H2O、LiNO3, salpeter solution and NH4H2PO4Ratio be 3.8mmol：
0.2mmol：0.4mmol：10mL：4mmol.
(3) mixed solution C is obtained with the pH=0.53 of dust technology regulation mixed solution B under agitation；
(4) above-mentioned mixed solution C is stirred into 60min, it is close in being transferred to band teflon-lined stainless steel cauldron
Envelope, after reacting 12h at 185 DEG C, naturally cools to room temperature；
(5) by the sediment centrifugation for obtaining (rotating speed is 10000r/min), centrifugation time is 5min, and with water and second
Alcohol repeated washing sediment, centrifugation is put in 80 DEG C of drying boxes after washing and is dried 10h, obtains the addition of hydro-thermal method synthesis
Li+Strengthen BiPO4:Sm3+The fluorescent material of luminescent properties.
Embodiment 4：
(1) 3.8mmol (1.843g) Bi (NO are taken3)3·5H2O、0.2mmol(0.089g)Sm(NO3)3·6H2O and
0.6mmol(0.041g)LiNO3Beaker mixing is put into, then is dissolved in the 10mL salpeter solutions that volume fraction is 13.4%,
Magnetic agitation 10min, obtains mixed solution A；
(2) 4mmolNH is weighed4H2PO4In being dissolved in 16mL deionized waters, stirring 28min is configured to 0.25mol/L's
NH4H2PO4Solution, is added dropwise in the mixed solution A obtained by step (1), stirs 20min, it is ensured that it is well mixed, and obtains
Mixed solution B；Wherein Bi (NO3)3、Sm(NO3)3·6H2O、LiNO3, salpeter solution and NH4H2PO4Ratio be 3.8mmol：
0.2mmol：0.6mmol：10mL：4mmol.
(3) mixed solution C is obtained with the pH=0.52 of dust technology regulation mixed solution B under agitation；
(4) above-mentioned mixed solution C is stirred into 40min, it is close in being transferred to band teflon-lined stainless steel cauldron
Envelope, after reacting 12.5h at 180 DEG C, naturally cools to room temperature；
(5) by the sediment centrifugation for obtaining (rotating speed is 10000r/min), centrifugation time is 5.5min, and with water and
Ethanol repeated washing sediment, centrifugation is put in 75 DEG C of drying boxes after washing and is dried 12h, obtains adding for hydro-thermal method synthesis
Plus Li+Strengthen BiPO4:Sm3+The fluorescent material of luminescent properties.
Embodiment 5：
(1) 3.8mmol (1.843g) Bi (NO are taken3)3·5H2O、0.2mmol(0.089g)Sm(NO3)3·6H2O and
1.0mmol(0.069g)LiNO3Beaker mixing is put into, then is dissolved in the 10mL salpeter solutions that volume fraction is 13.6%,
Magnetic agitation 12min, obtains mixed solution A；
(2) 4mmolNH is weighed4H2PO4In being dissolved in 10mL deionized waters, stirring 22min is configured to 0.4mol/L's
NH4H2PO4Solution, is added dropwise in the mixed solution A obtained by step (1), stirs 25min, it is ensured that it is well mixed, and obtains
Mixed solution B；Wherein Bi (NO3)3、Sm(NO3)3·6H2O、LiNO3, salpeter solution and NH4H2PO4Ratio be 3.8mmol：
0.2mmol：1.0mmol：10mL：4mmol.
(3) mixed solution C is obtained with the pH=0.55 of dust technology regulation mixed solution B under agitation；
(4) above-mentioned mixed solution C is stirred into 50min, it is close in being transferred to band teflon-lined stainless steel cauldron
Envelope, after reacting 13h at 181 DEG C, naturally cools to room temperature；
(5) by the sediment centrifugation for obtaining (rotating speed is 10000r/min), centrifugation time is 6min, and with water and second
Alcohol repeated washing sediment, centrifugation is put in 85 DEG C of drying boxes after washing and is dried 11h, obtains the addition of hydro-thermal method synthesis
Li+Strengthen BiPO4:Sm3+The fluorescent material of luminescent properties.
Jing is tested, the obtained Li of the present invention+Doping BiPO4:Sm3+Fluorescent material is monocline phase structure, and size is at 0.5～3 μm
Between.It is relatively free of addition Li+, its luminous intensity brings up to original 1.07～1.5 times, to developing BiPO4Base fluorescent material
It is significant.
One embodiment of the present invention is the foregoing is only, is not unique embodiment, this area scientific research, technology people
Member is the claim of the present invention by reading the present invention, any equivalent transformation done under without departing from this technical process
Covered.
Claims (10)
1. a kind of preparation method of lithium ion doped bismuth phosphate samarium fluorescent material, it is characterised in that：Comprise the following steps：
(1) Bi (NO are taken3)3·5H2O、Sm(NO3)3·6H2O and LiNO3It is added in salpeter solution after pressed powder mixing, stirs
Uniformly obtain mixed solution A；
(2) in mixed solution A NH is added dropwise again4H2PO4Solution, continues to stir until NH4H2PO4Solution fully dissolves, and is mixed
Close solution B；Wherein Bi (NO3)3·5H2O、Sm(NO3)3·6H2O、LiNO3And NH4H2PO4Ratio be 3.8mmol：0.2mmol：
xmmol：4mmol, x=0.1～1.0；
(3) pH value of mixed solution B is adjusted to 0.50～0.55, obtain mixed solution C；
(4) mixed solution C reacts generation precipitation at 180 DEG C～185 DEG C, when not increasing to precipitation, naturally cools to room temperature；
(5) the sediment centrifugation for obtaining step (4), the sediment being centrifugally separating to obtain is washed and is dried, and obtains lithium
Ion doping bismuth phosphate samarium fluorescent material.
2. the preparation method of a kind of lithium ion doped bismuth phosphate samarium fluorescent material according to claim 1, it is characterised in that：Step
Suddenly the volume fraction of salpeter solution is 13%～13.6% in (1)；NH in step (2)4H2PO4Solution is by NH4H2PO4Addition is gone
Stir in ionized water obtained in 20～30min, its concentration is 0.2～0.4mol/L；Salpeter solution and NH4H2PO4Ratio be
10mL：4mmol.
3. the preparation method of a kind of lithium ion doped bismuth phosphate samarium fluorescent material according to claim 1, it is characterised in that：Step
Suddenly 10～15min of stirring obtains mixed solution A in (1).
4. the preparation method of a kind of lithium ion doped bismuth phosphate samarium fluorescent material according to claim 1, it is characterised in that：Step
Suddenly 20～30min of stirring obtains mixed solution B in (2).
5. the preparation method of a kind of lithium ion doped bismuth phosphate samarium fluorescent material according to claim 1, it is characterised in that：Step
Suddenly in (4), mixed solution C first stirs 40～60min, is then transferred to be sealed in band teflon-lined stainless steel cauldron
Reaction.
6. the preparation method of a kind of lithium ion doped bismuth phosphate samarium fluorescent material according to claim 5, it is characterised in that：No
Rust steel reactor volume compactedness is 80%.
7. the preparation method of a kind of lithium ion doped bismuth phosphate samarium fluorescent material according to claim 1, it is characterised in that：Step
Suddenly 12～13h is reacted in (4).
8. the preparation method of a kind of lithium ion doped bismuth phosphate samarium fluorescent material according to claim 1, it is characterised in that：Step
Suddenly centrifugation is 5～6min of centrifugation under conditions of rotating speed is 10000r/min in (5)；Washing is to wash two with water
It is secondary, then washed once with ethanol.
9. the preparation method of a kind of lithium ion doped bismuth phosphate samarium fluorescent material according to claim 1, it is characterised in that：Step
Suddenly the drying in (5) is that 10～12h is dried in 75～85 DEG C of drying boxes.
10. lithium ion doped bismuth phosphate samarium fluorescent material obtained in the preparation method described in a kind of utilization claim 1, its feature exists
In：The lithium ion doped bismuth phosphate samarium fluorescent material is monocline phase structure, and size is between 0.5～3 μm.
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| WO2013094669A1 (en) * | 2011-12-22 | 2013-06-27 | 株式会社ジーシー | Agent for imparting fluorescence to ceramic |
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