CN104531152B - A kind of high-efficiency antioxidant method for annealing of rare earth fluoride luminescent material - Google Patents
A kind of high-efficiency antioxidant method for annealing of rare earth fluoride luminescent material Download PDFInfo
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- CN104531152B CN104531152B CN201410805371.7A CN201410805371A CN104531152B CN 104531152 B CN104531152 B CN 104531152B CN 201410805371 A CN201410805371 A CN 201410805371A CN 104531152 B CN104531152 B CN 104531152B
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Abstract
The high-efficiency antioxidant method for annealing of a kind of rare earth fluoride luminescent material belongs to solid luminescent material field.It is characterized in that comprising the steps of: be ground by rare earth fluoride fluorescent material, after crossing screen cloth, be directly compressed into biscuit body；Biscuit body is placed in alumina crucible, with quartz sand, biscuit body is buried and is filled up by alumina crucible；Being paved with activated carbon powder bottom the alumina crucible that another is bigger, be placed in big crucible by the crucible equipped with biscuit body built before, other space activated carbons of big crucible fill up, and build lid；The big crucible installed is placed in geneva stove and heats up with the heating rate of per hour 160 DEG C 200 DEG C, makes annealing treatment, be finally cooled to room temperature with stove after reaching annealing temperature.Fluoride light conversion agent crystallinity of the present invention is good, and has stronger upper conversion performance, effectively reduces the oxidized probability of fluoride and the generation of dephasign, improves the processing characteristics of fluoride rare earth material, reduce manufacturing cost.
Description
Technical field
The invention discloses the high-efficiency antioxidant method for annealing of a kind of rare earth fluoride luminescent material, belong to
Solid luminescent material field.
Background technology
Fluoride owing to having relatively low phonon energy, bigger band gap (～10eV) and from ultraviolet to red
Outer high transmitance, therefore often using it as the rear-earth-doped host material turning light.Prepare high saturating
Cross rate and having and well turn the pass that the rare-earth-doped fluoride light conversion agent of optical property is current device application
Key.
At present, people are concentrated mainly on N to the method for annealing of fluoride fluorescent material2Or Ar2Atmosphere is moved back
Fire, because annealing can form it into the impurity such as corresponding oxide and have a strong impact on its luminescence in atmosphere
Performance, but these method for annealing are higher to the requirement of equipment, and often due to vacuum not and
Sample is caused to be annealed unsuccessfully.This Technology for Heating Processing production efficiency is low and equipment cost and production cost
Higher, have a strong impact on the luminescent properties of fluoride fluorescent material.And the annealing side provided by the present invention
Method is simple to operation, and annealing simultaneously uniformly, decreases impact and the foreign material phase of other atmosphere such as oxygen
Generation, improve the quality of fluoride fluorescent material and enhance its luminescent properties, improving it and add
Work performance, reduces the production cost of fluoride fluorescent material.
Summary of the invention
It is an object of the invention to provide the high-efficiency antioxidant annealing side of a kind of rare earth fluoride luminescent material
Method.The features such as quartz sand quality is hard, fusing point is high, stable chemical nature are wherein make use of to be covered by sample
Lid, has used again the activated carbon absorption feature to oxygen and other impurity so that annealing process avoids
The impact of other atmosphere such as oxygen and the generation of foreign material phase.What method will obtain has certain degree of hardness
Fluoride biscuit body be placed in alumina crucible, buried with quartz sand and crucible filled up；?
Being paved with activated carbon powder bottom another bigger alumina crucible, the monkey before building is placed in
Wherein, other space activated carbons of big crucible fill up, and build lid；The crucible installing sample is put
Make annealing treatment at different temperatures in geneva stove, last furnace cooling.
The present invention is to provide the high-efficiency antioxidant method for annealing of a kind of rare earth fluoride luminescent material, bag
Include following steps:
Step one: be ground by prepared fluoride fluorescent material, is directly compressed into element after crossing screen cloth
Base substrate；
Step 2: the fluoride fluorescent material biscuit body obtained is placed in alumina crucible, with quartz
Sand is buried and is filled up by crucible；
Step 3: be paved with activated carbon powder bottom the alumina crucible that another is bigger, will build before
The crucible equipped with sample be placed in one, other space activated carbons of big crucible fill up, and build lid.
Step 4: the big crucible installed in step 3 is placed in geneva stove with per hour 160 DEG C-200 DEG C
Heating rate heat up, make annealing treatment after reaching annealing temperature, be finally cooled to room with stove
Temperature.
Directly can anneal in air atmosphere.
In step 2, use quartz sand, other impurity will not be introduced when annealing.
Use activated carbon cladding that sample in annealing process can be protected not oxidized in step 3.
The prepared crystallinity of fluoride fluorescent material, pattern, optical property are analyzed and contrast.
X-ray diffractometer is used to analyze its crystallinity；By its pattern of scanning electron microscope analysis；Optical
Can be tested by fluorescence spectrophotometer.
The present invention has the following advantages and benefit:
(1) method is simple, easily operates.Just can be at geneva stove for raw material with common quartz sand and carbon dust
In complete the annealing process of fluoride fluorescent material.Fluoride through different temperatures annealing turns light
Material crystalline is good, and has stronger upper conversion performance.
(2) the oxidized probability of fluoride and the generation of dephasign it are effectively reduced.
(3) improve the processing characteristics of fluoride rare earth material, reduce the life of fluoride fluorescent material
Produce manufacturing cost.
Accompanying drawing explanation
Fig. 1 is to use the method at the NaYF of 480 DEG C of annealing4: Yb3+, Ho3+XRD figure spectrum.
Fig. 2 is to use the method at the NaYF of 480 DEG C of annealing4: Yb3+, Ho3+Scanning electron microscope (SEM) photograph.
Fig. 3 is to use the method at the NaYF of 480 DEG C of annealing4: Yb3+, Ho3+At 980nm laser
Emission spectrum figure under exciting.
Fig. 4 is to use the method at the NaYF of 560 DEG C of annealing4: Yb3+, Ho3+XRD figure spectrum.
Fig. 5 is to use the method at the NaYF of 560 DEG C of annealing4: Yb3+, Ho3+Scanning electron microscope (SEM) photograph.
Fig. 6 is to use the method at the NaYF of 560 DEG C of annealing4: Yb3+, Ho3+At 980nm laser
Emission spectrum figure under exciting.
Fig. 7 is to use the method at the NaYF of 650 DEG C of annealing4: Yb3+, Ho3+XRD figure spectrum.
Fig. 8 is to use the method at the NaYF of 650 DEG C of annealing4: Yb3+, Ho3+Scanning electron microscope (SEM) photograph.
Fig. 9 is to use the method at the NaYF of 650 DEG C of annealing4: Yb3+, Ho3+At 980nm laser
Emission spectrum figure under exciting.
Figure 10 is to use the method at the YbF of 750 DEG C of annealing3: the XRD figure spectrum of Er3+.
Detailed description of the invention:
Further illustrating below by embodiment row near to the present invention, the present invention is by no means limited to be stated
Embodiment.
Embodiment 1:NaYF4: 20mol%Yb3+, 2mol%Ho3+Fluorescent material is 480 DEG C of employings
The annealing that the method for carbon cladding is carried out.
Weigh the NaYF using complex coprecipitation method to prepare4: Yb3+, Ho3+Powder 0.75g, at 5Mpa
Pressure under suppress 2min, obtain the plain idiosome of Φ 11.5mm.Element idiosome is placed in the oxygen of Φ 30mm
Change in aluminum crucible, buried with quartz sand and crucible is filled up, at the bottom of the alumina crucible of Φ 60mm
Portion is paved with activated carbon powder, is placed in one by the crucible of the Φ 30mm built, other of Φ 60mm crucible
Space activated carbon fills up, and builds lid.Geneva stove is warming up to the heating rate of 3 DEG C per minute
480 DEG C, it is incubated 4h, afterwards furnace cooling.Its XRD figure spectrum is shown in that figure is shown in by Fig. 1, SEM collection of illustrative plates, 2,
Emission spectrum figure under 980nm laser excitation is shown in Fig. 3.
Embodiment 2:NaYF4: 20mol%Yb3+, 2mol%Ho3+Fluorescent material uses carbon at 480 DEG C
The annealing that the method for cladding is carried out.
Weigh the NaYF using complex coprecipitation method to prepare4: Yb3+, Ho3+Powder 0.75g, at 5Mpa
Pressure under suppress 2min, obtain the plain idiosome of Φ 11.5mm.Element idiosome is placed in the oxygen of Φ 30mm
Change in aluminum crucible, buried with quartz sand and crucible is filled up, at the bottom of the alumina crucible of Φ 60mm
Portion is paved with activated carbon powder, is placed in one by the crucible of the Φ 30mm built, other of Φ 60mm crucible
Space activated carbon fills up, and builds lid.Geneva stove is warming up to the heating rate of 3 DEG C per minute
560 DEG C, it is incubated 4h, afterwards furnace cooling.Its XRD figure spectrum is shown in that Fig. 4, SEM collection of illustrative plates is shown in Fig. 5, at 980nm
Emission spectrum figure under laser excitation is shown in Fig. 6.
Embodiment 3:NaYF4: 20mol%Yb3+, 2mol%Ho3+Fluorescent material uses carbon at 680 DEG C
The annealing that the method for cladding is carried out.
Weigh the NaYF using complex coprecipitation method to prepare4: Yb3+, Ho3+Powder 0.75g, at 5Mpa
Pressure under suppress 2min, obtain the plain idiosome of Φ 11.5mm.Element idiosome is placed in the oxygen of Φ 30mm
Change in aluminum crucible, buried with quartz sand and crucible is filled up, at the bottom of the alumina crucible of Φ 60mm
Portion is paved with activated carbon powder, is placed in one by the crucible of the Φ 30mm built, other of Φ 60mm crucible
Space activated carbon fills up, and builds lid.Geneva stove is warming up to the heating rate of 3 DEG C per minute
680 DEG C, it is incubated 4h, afterwards furnace cooling.Its XRD figure spectrum is shown in that Fig. 7, SEM collection of illustrative plates is shown in Fig. 8, at 980nm
Emission spectrum figure under laser excitation is shown in Fig. 9.
Embodiment 4:YbF3: 10%Er fluorescent powder material is carried out 750 DEG C of methods using carbon cladding
Annealing.
Weigh the YbF using solid-phase synthesis to prepare3: 10%Er powder 0.75g, under the pressure of 5Mpa
Compacting 2min, obtains the plain idiosome of Φ 11.5mm.Element idiosome is placed in the alumina crucible of Φ 30mm
In, buried with quartz sand and crucible is filled up, bottom the alumina crucible of Φ 60mm, being paved with work
Property powdered carbon, the crucible of the Φ 30mm built is placed in one, live in other spaces of Φ 60mm crucible
Property charcoal fills up, and builds lid.It is warming up to 750 DEG C with the heating rate of 3 DEG C per minute in geneva stove,
Insulation 4h, afterwards furnace cooling.Its XRD figure spectrum is shown in Figure 10.
Claims (1)
1. the high-efficiency antioxidant method for annealing of a rare earth fluoride fluorescent material, it is characterised in that
Comprise the steps of:
Step one: be ground by rare earth fluoride fluorescent material, is directly compressed into after crossing screen cloth
Biscuit body；
Step 2: be placed in alumina crucible by the biscuit body obtained, with quartz sand by biscuit body
Bury and alumina crucible is filled up；
Step 3: at another the biggest crucible of bigger alumina crucible, big crucible
Bottom is paved with activated carbon powder, is placed in big crucible by the crucible equipped with biscuit body built before,
Other space activated carbons of big crucible fill up, and build lid；
Step 4: the big crucible installed in step 3 is placed in geneva stove with per hour 160 DEG C
The heating rate of-200 DEG C heats up, and makes annealing treatment after reaching annealing temperature, finally with
Stove is cooled to room temperature.
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| FR2554121B1 (en) * | 1983-11-02 | 1985-12-06 | Rhone Poulenc Spec Chim | NOVEL "ANTI-STOKES" LUMINESCENT SUBSTANCES, THEIR MANUFACTURING PROCESS AND THEIR APPLICATION IN ANY SYSTEM USING LUMINESCENCE IN THE SPECTRAL REGION CONCERNED |
| CN102660801B (en) * | 2012-02-24 | 2013-12-25 | 长春理工大学 | Method for preparing erbium and ytterbium double-doped yttrium lithium tetrafluoride up-conversion luminescent nanobelt |
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