CN110041933A - A kind of Bi3+Doping enhancing Ce3+The fluorescent powder of yellow emission - Google Patents
A kind of Bi3+Doping enhancing Ce3+The fluorescent powder of yellow emission Download PDFInfo
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Abstract
A kind of Bi3+Doping enhancing Ce3+The fluorescent powder of yellow emission.The invention discloses a kind of Bi3+Doping enhancing Ce3+(Gd, Y) AG fluorescent powder of yellow emission, chemical constitution formula are (Gd0.74Y0.2Bi0.05Ce0.01)3Al5O12((Gd0.74Y0.2Bi0.05Ce0.01)AG).This is that the synthetic method of fluorescent powder is stoichiometrically to be mixed into female salting liquid with rare earth nitrate solution and aluminum nitrate solution, to obtain suspension after ammonium bicarbonate precipitation agent mixing, and by centrifugation, washing, the white presoma of dry acquisition, (Gd finally is obtained through calcining0.74Y0.2Bi0.05Ce0.01) AG yellow fluorescent powder.Fluorescent powder preparation method prepared by the present invention is simple, pattern uniformly, good dispersion, fluorescence property it is excellent.
Description
Technical field
The present invention relates to a kind of fluorescent powders and preparation method applied to the fields such as illumination and display.
Background technique
An important branch of the gadolinium aluminate-base fluorescent material as phosphor is widely used in LED illumination
And the fields such as display, imaging of medical.Development however as technology of preparing and the progress of science and technology, traditional fluorescent material by
It is not able to satisfy the demand of people gradually.
The microscopic appearance that (Gd, Y) AG fluorescent powder has monodisperse, pattern uniform, and Gd3+And Bi3+It is quick well again
Agent can enhance Ce3+Yellow emission.Therefore, this yellow fluorescent powder is developed to have very important significance.
Summary of the invention
The present invention is directed to propose a kind of Bi in view of the deficiency of the prior art3+/Ce3+Codope (Gd, Y) AG is novel
Yellow fluorescent powder.
Technical problem to be solved by the invention is to provide one kind (Gd0.74Y0.2Bi0.05Ce0.01) AG fluorescent powder, the fluorescence
Powder has a clear superiority compared with conventional fluorescent powder: a) (Gd0.74Y0.2Bi0.05Ce0.01) AG fluorescent powder have good monodispersity and
Uniform pattern, fluorescence property are good;B) in Gd3+To Bi3+And Bi3+To Ce3+Between energy transmission on the basis of, Ce3+Huang
Light emitting further enhances, to improve fluorescence property.
To achieve the above object, the present invention takes following scheme:
A kind of Bi3+Doping enhancing Ce3+The fluorescent powder of yellow emission, preparation method the following steps are included:
(1) by powdery rare earth oxide (Gd2O3、Y2O3And CeO2) be dissolved in appropriate nitric acid solution, it dissolves by heating and removed
The nitric acid of amount, is made into rare earth nitrate solution;
(2) (Gd is pressed0.75-x Y0.2Bi0.05Ce x )3Al5O12Stoichiometric ratio measures rare earth nitrades, Bi (NO3)3With Al (NO3)3
Solution is mixed, and deionized water is added and is made into the solution that volume is 100 mL, stirs 10 min, keeps female salting liquid mixing equal
It is even;
(3) appropriate NH is weighed4HCO3It is dissolved in deionized water, is placed in thermostat water bath, temperature is adjusted and is stirred for 25 DEG C
It mixes, until NH4HCO3Dissolution;
(4) mixed liquor obtained by step (2) is injected in pyriform funnel, at room temperature by female salting liquid with 5 mL/min's
Speed instills NH4HCO3In precipitant solution, reaction obtains suspension, and 30 min are stirred after titration and carry out ageing treatment;
(5) by suspension obtained by step (4) through centrifugation, clean, be dried to obtain white precursor powder;
(6) by precursor powder obtained by step (5) through 1500 DEG C of 4 h of calcining and in Ar/H2It is fired under atmosphere
1000 DEG C and heat preservation 4 h, final acquisition (Gd0.8-x Y0.2Bi0.05Ce x )3Al5O12Fluorescent powder.
Detailed description of the invention
Fig. 1 is through (Gd obtained by 1500 DEG C of calcinings0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.01) yellow fluorescent powder XRD diagram
Spectrum.
Fig. 2 is through (Gd obtained by 1500 DEG C of calcinings0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.01) yellow fluorescent powder SEM schemes
Spectrum.
Fig. 3 is through (Gd obtained by 1500 DEG C of calcinings0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.01) fluorescent powder is in 465 nm
Emission spectrum under excitation;Embedded figure is 574 nm fluorescence intensities with Ce contentxThe curve of variation.
Below by specific examples comparative, the present invention is further explained.
Preferred example:
A kind of Bi3+Doping enhancing Ce3+The fluorescent powder of yellow emission, the preparation method is as follows:
It is raw materials used: Gd2O3(99.99%), Y2O3(99.99%), CeO2(99.99%), Bi (NO3)3·5H2O (99.0%), Al
(NO3)3·9H2O (99.0%), NH4HCO3(99.0%), nitric acid (HNO3, 68%);
(1) by powdery Gd2O3、Y2O3And CeO2It is dissolved in hot nitric acid respectively, removes excess HNO3It is made into rare earth nitrate solution
;
(2) (Gd is pressed0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.01) stoichiometric ratio measures rare earth nitrades, Bi (NO3)3
Solution and Al (NO3)3Solution is added deionized water and is made into the solution that volume is 100 mL, stirs 10 min, keep female salting liquid equal
Even mixing;
(3) appropriate NH is weighed4HCO3It is dissolved in deionized water, is placed in thermostat water bath, temperature is adjusted and is stirred for 25 DEG C
It mixes, until NH4HCO3Dissolution;
(4) mixed liquor obtained by step (2) is injected in pyriform funnel, at room temperature by female salting liquid with 5 mL/min's
Speed instills NH4HCO3It is reacted to obtain suspension in solution, stirring is continued to suspension after to be titrated and is carried out at timeliness
Reason, time are 30 min;
(5) by suspension obtained by step (4) through centrifugation, cleaning, the white precursor powder of dry acquisition;
(6) by precursor powder obtained by step (5) through 1500 DEG C of 4 h of calcining, and in Ar/H2It is fired under atmosphere
1000 DEG C and heat preservation 4 h, final acquisition (Gd0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.01) fluorescent powder.
Embodiment 2
A kind of Bi3+Doping enhancing Ce3+The fluorescent powder of yellow emission, the preparation method is as follows:
It is raw materials used: Gd2O3(99.99%), Y2O3(99.99%), CeO2(99.99%), Bi (NO3)3·5H2O (99.0%), Al
(NO3)3·9H2O (99.0%), NH4HCO3(99.0%), nitric acid (HNO3, 68%);
(1) by powdery Gd2O3、Y2O3And CeO2It is dissolved in hot nitric acid respectively, removes excess HNO3It is made into rare earth nitrate solution
;
(2) (Gd is pressed0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.001) stoichiometric ratio measures rare earth nitrades, Bi (NO3)3
Solution and Al (NO3)3Solution is added deionized water and is made into the solution that volume is 100 mL, stirs 10 min, keep female salting liquid equal
Even mixing;
(3) appropriate NH is weighed4HCO3It is dissolved in deionized water, is placed in thermostat water bath, temperature is adjusted and is stirred for 25 DEG C
It mixes, until NH4HCO3Dissolution;
(4) mixed liquor obtained by step (2) is injected in pyriform funnel, at room temperature by female salting liquid with 5 mL/min's
Speed instills NH4HCO3It is reacted to obtain suspension in solution, stirring is continued to suspension after to be titrated and is carried out at timeliness
Reason, time are 30 min;
(5) by suspension obtained by step (4) through centrifugation, cleaning, the white precursor powder of dry acquisition;
(6) by precursor powder obtained by step (5) through 1500 DEG C of 4 h of calcining, and in Ar/H2It is fired under atmosphere
1000 DEG C and heat preservation 4 h, final acquisition (Gd0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.001) fluorescent powder.
Embodiment 3
A kind of Bi3+Doping enhancing Ce3+The fluorescent powder of yellow emission, the preparation method is as follows:
It is raw materials used: Gd2O3(99.99%), Y2O3(99.99%), CeO2(99.99%), Bi (NO3)3·5H2O (99.0%), Al
(NO3)3·9H2O (99.0%), NH4HCO3(99.0%), nitric acid (HNO3, 68%);
(1) by powdery Gd2O3、Y2O3And CeO2It is dissolved in hot nitric acid respectively, removes excess HNO3It is made into rare earth nitrate solution
;
(2) (Gd is pressed0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.003) stoichiometric ratio measures rare earth nitrades, Bi (NO3)3
Solution and Al (NO3)3Solution is added deionized water and is made into the solution that volume is 100 mL, stirs 10 min, keep female salting liquid equal
Even mixing;
(3) appropriate NH is weighed4HCO3It is dissolved in deionized water, is placed in thermostat water bath, temperature is adjusted and is stirred for 25 DEG C
It mixes, until NH4HCO3Dissolution;
(4) mixed liquor obtained by step (2) is injected in pyriform funnel, at room temperature by female salting liquid with 5 mL/min's
Speed instills NH4HCO3It is reacted to obtain suspension in solution, stirring is continued to suspension after to be titrated and is carried out at timeliness
Reason, time are 30 min;
(5) by suspension obtained by step (4) through centrifugation, cleaning, the white precursor powder of dry acquisition;
(6) by precursor powder obtained by step (5) through 1500 DEG C of 4 h of calcining, and in Ar/H2It is fired under atmosphere
1000 DEG C and heat preservation 4 h, final acquisition (Gd0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.003) fluorescent powder.
Embodiment 4
A kind of Bi3+Doping enhancing Ce3+The fluorescent powder of yellow emission, the preparation method is as follows:
It is raw materials used: Gd2O3(99.99%), Y2O3(99.99%), CeO2(99.99%), Bi (NO3)3·5H2O (99.0%), Al
(NO3)3·9H2O (99.0%), NH4HCO3(99.0%), nitric acid (HNO3, 68%);
(1) by powdery Gd2O3、Y2O3And CeO2It is dissolved in hot nitric acid respectively, removes excess HNO3It is made into rare earth nitrate solution
;
(2) (Gd is pressed0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.005) stoichiometric ratio measures rare earth nitrades, Bi (NO3)3
Solution and Al (NO3)3Solution is added deionized water and is made into the solution that volume is 100 mL, stirs 10 min, keep female salting liquid equal
Even mixing;
(3) appropriate NH is weighed4HCO3It is dissolved in deionized water, is placed in thermostat water bath, temperature is adjusted and is stirred for 25 DEG C
It mixes, until NH4HCO3Dissolution;
(4) mixed liquor obtained by step (2) is injected in pyriform funnel, at room temperature by female salting liquid with 5 mL/min's
Speed instills NH4HCO3It is reacted to obtain suspension in solution, stirring is continued to suspension after to be titrated and is carried out at timeliness
Reason, time are 30 min;
(5) by suspension obtained by step (4) through centrifugation, cleaning, the white precursor powder of dry acquisition;
(6) by precursor powder obtained by step (5) through 1500 DEG C of 4 h of calcining, and in Ar/H2It is fired under atmosphere
1000 DEG C and heat preservation 4 h, final acquisition (Gd0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.005) fluorescent powder.
Embodiment 5
A kind of Bi3+Doping enhancing Ce3+The fluorescent powder of yellow emission, the preparation method is as follows:
It is raw materials used: Gd2O3(99.99%), Y2O3(99.99%), CeO2(99.99%), Bi (NO3)3·5H2O (99.0%), Al
(NO3)3·9H2O (99.0%), NH4HCO3(99.0%), nitric acid (HNO3, 68%);
(1) by powdery Gd2O3、Y2O3And CeO2It is dissolved in hot nitric acid respectively, removes excess HNO3It is made into rare earth nitrate solution
;
(2) (Gd is pressed0.75-x Y0.2Bi0.005Ce x )3Al5O12 (x=0.007) stoichiometric ratio measures rare earth nitrades, Bi (NO3)3
Solution and Al (NO3)3Solution is added deionized water and is made into the solution that volume is 100 mL, stirs 10 min, keep female salting liquid equal
Even mixing;
(3) appropriate NH is weighed4HCO3It is dissolved in deionized water, is placed in thermostat water bath, temperature is adjusted and is stirred for 25 DEG C
It mixes, until NH4HCO3Dissolution;
(4) mixed liquor obtained by step (2) is injected in pyriform funnel, at room temperature by female salting liquid with 5 mL/min's
Speed instills NH4HCO3It is reacted to obtain suspension in solution, stirring is continued to suspension after to be titrated and is carried out at timeliness
Reason, time are 30 min;
(5) by suspension obtained by step (4) through centrifugation, cleaning, the white precursor powder of dry acquisition;
(6) by precursor powder obtained by step (5) through 1500 DEG C of 4 h of calcining, and in Ar/H2It is fired under atmosphere
1000 DEG C and heat preservation 4 h, final acquisition (Gd0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.007) fluorescent powder.
Embodiment 6
A kind of Bi3+Doping enhancing Ce3+The fluorescent powder of yellow emission, the preparation method is as follows:
It is raw materials used: Gd2O3(99.99%), Y2O3(99.99%), CeO2(99.99%), Bi (NO3)3·5H2O (99.0%), Al
(NO3)3·9H2O (99.0%), NH4HCO3(99.0%), nitric acid (HNO3, 68%);
(1) by powdery Gd2O3、Y2O3And CeO2It is dissolved in hot nitric acid respectively, removes excess HNO3It is made into rare earth nitrate solution
;
(2) (Gd is pressed0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.02) stoichiometric ratio measures rare earth nitrades, Bi (NO3)3
Solution and Al (NO3)3Solution is added deionized water and is made into the solution that volume is 100 mL, stirs 10 min, keep female salting liquid equal
Even mixing;
(3) appropriate NH is weighed4HCO3It is dissolved in deionized water, is placed in thermostat water bath, temperature is adjusted and is stirred for 25 DEG C
It mixes, until NH4HCO3Dissolution;
(4) mixed liquor obtained by step (2) is injected in pyriform funnel, at room temperature by female salting liquid with 5 mL/min's
Speed instills NH4HCO3It is reacted to obtain suspension in solution, stirring is continued to suspension after to be titrated and is carried out at timeliness
Reason, time are 30 min;
(5) by suspension obtained by step (4) through centrifugation, cleaning, the white precursor powder of dry acquisition;
(6) by precursor powder obtained by step (5) through 1500 DEG C of 4 h of calcining, and in Ar/H2It is fired under atmosphere
1000 DEG C and heat preservation 4 h, final acquisition (Gd0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.02) fluorescent powder.
Claims (9)
1. a kind of Bi3+Doping enhancing Ce3+The fluorescent powder of yellow emission, it is characterised in that including chemical constitution formula be (Gd0.8-x- y Y0.2Bi0.05Ce x )3Al5O12Component,xValue is 0.01, and wherein luminous host material is 20 at.% Y3+Doping
Gd3Al5O12。
2. a kind of Bi3+Doping enhancing Ce3+The fluorescent powder of yellow emission, which comprises the following steps:
(1) by rare earth oxide (Gd2O3、Y2O3And CeO2) be dissolved in hot nitric acid and be configured to rare earth nitrate solution, by appropriate Bi
(NO3)3It is dissolved in dust technology and is made into Bi (NO3)3Solution, by appropriate Al (NO3)3It is dissolved in deionized water and is made into Al (NO3)3Solution;
(2) Gd is pressed3+: Y3+: Bi3+: Ce3+Molar ratio 0.75-x: 0.2: 0.05: x (x=0.01) nitrate solution is measured,
With the Al (NO stoichiometrically measured3)3Solution is mixed, and deionized water is added and is made into the solution that volume is 100 ml, into
Row stirring, is uniformly mixed female salting liquid;
(3) suitable ammonium hydrogen carbonate (NH is weighed4HCO3) particle is dissolved in deionized water, it is made into the precipitant solution of 160 ml, is placed in
25 oIt is stirred evenly in C magnetic stirring apparatus, until NH4HCO3Particle is completely dissolved;
(4) female salting liquid that step (2) prepares at the uniform velocity is instilled into the NH that step (3) prepares by pear shape separatory funnel4HCO3Precipitating
In agent solution, reaction obtains white suspension, continues stirring after to be titrated and carries out ageing treatment,;
(5) mixed liquor that step (4) obtains is centrifuged by centrifuge, collects precipitating, and with deionized water and anhydrous
Ethyl alcohol repeatedly washs precipitating, finally dries at 80 DEG C, obtains white precursor powder;
(6) presoma obtained by step (5) is calcined 4 hours at 1500 DEG C, and restored in a hydrogen atmosphere, finally obtained
(Gd0.75-x Y0.2Bi0.05Ce x )3Al5O12 (x=0.01) fluorescent powder.
3. preparation method as claimed in claim 2, which is characterized in that cation concn is 0.24 M.
4. preparation method as claimed in claim 2, which is characterized in that selected precipitating reagent is NH4HCO3Solution, dosage are
160 mL, concentration used are 1.5 M.
5. preparation method as claimed in claim 2, which is characterized in that female salt mixing time is 10 min.
6. preparation method as claimed in claim 2, which is characterized in that female salt rate of titration is 5 mL/min.
7. preparation method as claimed in claim 2, which is characterized in that aging time is 30 min.
8. preparation method as claimed in claim 2, which is characterized in that presoma is respectively with deionized water cleaning 2 times, with ethyl alcohol
Cleaning 1 time.
9. preparation method as claimed in claim 2, which is characterized in that presoma calcining is divided into two stages, first in air
It is fired to 1500 DEG C under atmosphere, keeps the temperature 4 h;Afterwards in Ar/H2 (20 vol.% H2) 1000 DEG C are fired under atmosphere, heat preservation
4h。
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Cited By (1)
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CN114477266A (en) * | 2022-02-11 | 2022-05-13 | 包头稀土研究院 | Method for improving near infrared reflectivity of yellow pigment |
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CN114477266A (en) * | 2022-02-11 | 2022-05-13 | 包头稀土研究院 | Method for improving near infrared reflectivity of yellow pigment |
CN114477266B (en) * | 2022-02-11 | 2024-01-23 | 包头稀土研究院 | Method for improving near infrared reflectivity of yellow pigment |
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Application publication date: 20190723 |