CN105112054B - A kind of Tb3+Adulterate yttrium aluminmiu garnet new phosphorses - Google Patents
A kind of Tb3+Adulterate yttrium aluminmiu garnet new phosphorses Download PDFInfo
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- CN105112054B CN105112054B CN201510521378.0A CN201510521378A CN105112054B CN 105112054 B CN105112054 B CN 105112054B CN 201510521378 A CN201510521378 A CN 201510521378A CN 105112054 B CN105112054 B CN 105112054B
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Abstract
The invention discloses a kind of Tb3+Yttrium aluminmiu garnet new phosphorses are adulterated, its chemical constitution formula is (Gd0.9Tb0.1)3Al5O12(GdAG:Tb3+).This is that the synthetic method of fluorescent material is with rare earth nitrades and Al (NO3)3Solution is stoichiometrically mixed as female salting liquid, with NH4HCO3For precipitating reagent, suspension is obtained by reverse sluggish precipitation.On this basis, by centrifuging, cleaning, the dry white precursor powder of acquisition, finally GdAG is obtained through calcining:Tb3+New phosphorses.Fluorescent phosphor excellent performance prepared by the present invention, it is expected to turn into a new generation's illumination display material.
Description
Technical field
The present invention relates to a kind of fluorescent material and preparation method for being applied to the field such as illumination and display.
Background technology
Light emitting diode (LED) is used as a kind of novel green cold light source, has small volume, luminous intensity height, uses electrical power consumed
The advantages that small and long lifespan, it is widely used in illuminating, shows and the numerous areas such as traffic lights.With embedded photoluminescent material
Constantly update and the popularization and development of LED technology, traditional LED light source can not gradually meet the needs of people are growing.
YAG (the Y being widely used at present3Al5O12) it is fluorescent material (such as YAG:Tb3+Fluorescent material), energy conversion effect be present
The problems such as rate is low, and luminous intensity is not high, and product granularity is uneven, so as to limit the development of LED technology.Therefore it is glimmering in YAG systems
It is significant that a kind of novel high-quality fluorescent material is developed on the basis of light powder.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of GdAG:Tb3+Green high-efficient fluorescent material and preparation method, should
The more traditional YAG systems fluorescent material of fluorescent material has a clear superiority：A) yttrium aluminmiu garnet (Gd3Al5O12, GdAG) and there is thermally labile
Property, 10%atTb doping GdAG can stablize its lattice, remain to obtain the pomegranate of stable lattice when calcining heat reaches 1500 DEG C
Stone pure phase；b）The position in the periodic table of elements is adjacent with Tb by Gd, and+trivalent ionic radius is more or less the same, and this causes Tb3+Substitute Gd3+
Distortion of lattice is small caused by case, effectively reduces the generation of lattice defect, so as to improve luminous intensity to greatest extent；c）
Gd3+Tb can be sensitized3+Green emission, so as to strengthen fluorescence property；d）Gd (157) atomic weight is close to Tb (159) and remote high
In Y (89) so that this is that novel fluorescent material has higher solid density, and power is prevented so as to effectively improve its radiation
Degree, it is preferably to be used for scintillator material.
To achieve the above object, the present invention takes following scheme：
A kind of Tb3+Yttrium aluminmiu garnet new phosphorses are adulterated, preparation method comprises the following steps：
(1) by powdery rare earth oxide（Gd2O3And Tb4O7）It is dissolved in appropriate salpeter solution, dissolves by heating and removed
The nitric acid of amount, is made into rare earth nitrate solution；
(2) (Gd is pressed0.9Tb0.1)3Al5O12Stoichiometric proportion, measure rare earth nitrades, Al (NO3)3Solution is mixed,
Add deionized water and be made into the solution that volume is 100mL, be stirred, be well mixed female salting liquid；
(3) appropriate NH is weighed4HCO3Deionized water is dissolved in, is placed in thermostat water bath, regulation temperature is 25 DEG C and stirred
Mix, until NH4HCO3Dissolving；
(4) by mixed liquor injection pyriform funnel obtained by step (2), female salting liquid is instilled into NH at room temperature4HCO3Precipitation
In agent solution, reaction obtains suspension, and titration continues stirring and carries out Ageing Treatment after terminating；
(5) by suspension obtained by step (4) through centrifuging, cleaning, being dried to obtain white precursor powder；
(6) by precursor powder obtained by step (5) through 600 DEG C of calcining 4h and in Ar/H21300 are fired under atmosphere respectively
DEG C and 1500 DEG C, be incubated 2h, finally obtain GdAG:Tb3+New phosphorses.
Brief description of the drawings
Fig. 1 calcines gained (Gd through different temperatures0.9Tb0.1)3Al5O12The XRD spectrum of green emitting phosphor.
Fig. 2 is through 1300 DEG C of calcining gained (Gd0.9Tb0.1)3Al5O12The emission spectrum of green emitting phosphor.
Below by specific example, the present invention is expanded on further.
Embodiment 1
A kind of Tb3+Yttrium aluminmiu garnet new phosphorses are adulterated, preparation method is as follows：
It is raw materials used：Gd2O3(99.99%), Tb4O7(99.99%), Al (NO3)3·9H2O (99.0%), NH4HCO3
(99.0%), nitric acid (HNO3, 68%)；
(1) by powdery Gd2O3And Tb4O7It is dissolved in respectively in hot nitric acid, removes excessive HNO3It is made into rare earth nitrate solution；
(2) Gd is pressed3+:Tb3+:Al3+Mol ratio 2.7: 0.3:5 measure rare earth nitrades, Al (NO3)3Solution, addition go from
Sub- water is made into the solution that volume is 100mL, stirs 30min, female salting liquid is uniformly mixed；
(3) appropriate NH is weighed4HCO3Deionized water is dissolved in, is placed in thermostat water bath, regulation temperature is 25 DEG C and stirred
Mix, until NH4HCO3Dissolving；
(4) mixed liquor obtained by step (2) is injected in pyriform funnel, at room temperature by female salting liquid with 5mL/min speed
Degree instills NH4HCO3It is reacted to obtain suspension in solution, continue stirring after end to be titrated to suspension and carry out Ageing Treatment,
Time is 30min；
(5) by suspension obtained by step (4) through centrifuging, cleaning, the dry white precursor powder of acquisition；
(6) by precursor powder obtained by step (5) through 600 DEG C of calcining 4h and in Ar/H21300 are fired under atmosphere respectively
DEG C and 1500 DEG C, be incubated 2h, finally obtain GdAG:Tb3+New phosphorses.
Embodiment 2
A kind of new garnet-base efficient green fluorescent material, preparation method are as follows：
It is raw materials used：Gd2O3(99.99%), Tb4O7(99.99%), Al (NO3)3·9H2O (99.0%), NH4HCO3
(99.0%), nitric acid (HNO3, 68%)；
(1) by powdery Gd2O3And Tb4O7It is dissolved in respectively in hot nitric acid, removes excessive HNO3It is made into rare earth nitrate solution；
(2) Gd is pressed3+:Tb3+:Al3+Mol ratio 2.7: 0.3:5 measure rare earth nitrades, Al (NO3)3Solution, addition go from
Sub- water is made into the solution that volume is 100mL, stirs 30min, female salting liquid is uniformly mixed；
(3) appropriate NH is weighed4HCO3Deionized water is dissolved in, is placed in thermostat water bath, regulation temperature is 25 DEG C and stirred
Mix, until NH4HCO3Dissolving；
(4) mixed liquor obtained by step (2) is injected in pyriform funnel, at room temperature by female salting liquid with 5mL/min speed
Degree instills NH4HCO3It is reacted to obtain suspension in solution, continue stirring after end to be titrated to suspension and carry out Ageing Treatment,
Time is 30min；
(5) by suspension obtained by step (4) through centrifuging, cleaning, the dry white precursor powder of acquisition；
(6) by precursor powder obtained by step (5) through 600 DEG C of calcining 4h and in Ar/H21300 are fired under atmosphere respectively
DEG C and 1500 DEG C, be incubated 2h, finally obtain GdAG:Tb3+New phosphorses.
Fig. 1 is calcining gained (Gd under different temperatures0.9Tb0.1)3Al5O12The XRD spectrum of fluorescent material.As seen from the figure, pass through
Gained fluorescent material is garnet pure phase after 1300 DEG C and 1500 DEG C calcinings, and with the rise of calcining heat, XRD can be observed
Diffraction peak intensity increase, peak shape are more sharp, and this explanation crystal grain is constantly grown up with temperature rise.In this process, no thermal decomposition row
For this explanation 10%atTb3+The stabilisation of GdAG crystal structures, and GdAG can be achieved in addition:Tb3+With stable lattice knot
Structure.
Fig. 2 is that (Gd obtained by 4h is calcined at 1300 DEG C0.9Tb0.1)3Al5O12The emission spectrum of fluorescent material.As seen from the figure, exist
275nm is excited down, and a series of emission peaks occurs in emission spectrum, respectively at ~ 545nm5D4→7F5Transition（Green glow）、~
At 490nm5D4→7F6Transition（Blue light）And at 589nm5D4→7F4At transition and 625nm5D4→7F3Transition（Feux rouges）.
Emission spectrum peak shape at 545nm is sharp, and has highest emissive porwer, it was demonstrated that the fluorescent material has excellent green glow hair
Penetrate.
Claims (5)
- A kind of 1. Tb3+Adulterate the preparation method of yttrium aluminmiu garnet new phosphorses, it is characterised in that the chemical group of the fluorescent material An accepted way of doing sth is (Gd0.9Tb0.1)3Al5O12, comprise the following steps：(1) by rare earth oxide Gd2O3And Tb4O7It is dissolved in hot nitric acid and is made into rare earth nitrate solution, by appropriate Al (NO3)3It is dissolved in Deionized water is made into Al (NO3)3Solution；(2) Gd is pressed3+:Tb3+:Al3+Mol ratio 2.7:0.3:5, measure rare earth nitrades, Al (NO3)3Solution is mixed, and is added Deionized water is made into the solution that volume is 100mL, is stirred, is well mixed female salting liquid, rare earth ion concentration is 0.09M；(3) appropriate NH is weighed4HCO3Deionized water is dissolved in, is placed in thermostat water bath, regulation temperature is 25 DEG C, is stirred, directly To NH4HCO3It is completely dissolved；(4) by mixed liquor injection pyriform funnel obtained by step (2), female salting liquid is instilled into NH at room temperature4HCO3Precipitating reagent is molten In liquid, reaction obtains suspension, and titration continues stirring and carries out Ageing Treatment after terminating；(5) by suspension obtained by step (4) through centrifuging, cleaning, being dried to obtain white precursor powder；(6) precursor powder obtained by step (5) is through calcining final acquisition GdAG:Tb3+New phosphorses；Presoma calcining is divided into two In the individual stage, it is fired to 600 DEG C in air atmosphere first, is incubated 4h；Afterwards respectively in H2Volume fraction is 5% Ar and H2Mixing 1300 DEG C and 1500 DEG C are fired under atmosphere, are incubated 2h.
- 2. preparation method as claimed in claim 1, it is characterised in that selected precipitating reagent is NH4HCO3, dosage is 160mL, concentration used are 1.5M.
- 3. preparation method as claimed in claim 1, it is characterised in that female salt mixing time is 30min.
- 4. preparation method as claimed in claim 1, it is characterised in that female salt rate of titration is 5mL/min.
- 5. preparation method as claimed in claim 1, it is characterised in that aging time 30min.
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| CN111253073A (en) * | 2020-01-21 | 2020-06-09 | 徐州凹凸光电科技有限公司 | Method for preparing gadolinium-aluminum-garnet-based white-light glass ceramic by adopting sol-gel method |
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| CN100347267C (en) * | 2005-03-21 | 2007-11-07 | 南昌大学 | Garnet type gadolinium aluminate based fluorescent powder and method for making same |
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Inventor after: Li Jinkai Inventor after: Teng Xin Inventor after: Liu Zongming Inventor after: Duan Guangbin Inventor before: Teng Xin Inventor before: Li Jinkai Inventor before: Liu Zongming Inventor before: Duan Guangbin Inventor before: Hou Qingyue |
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Application publication date: 20151202 Assignee: SHANDONG PUTAI ENGINEERING TESTING AND IDENTIFICATION Co.,Ltd. Assignor: University of Jinan Contract record no.: X2020980002869 Denomination of invention: A new type Tb3+doped gadolinium aluminum garnet phosphor Granted publication date: 20171212 License type: Exclusive License Record date: 20200608 |
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