CN107573936A - A kind of zirconia solid solution base up-conversion luminescence powder material and preparation method thereof - Google Patents
A kind of zirconia solid solution base up-conversion luminescence powder material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to up-conversion luminescent material field, specially a kind of zirconia solid solution base infrared up conversion luminescent powder material and preparation method thereof.The chemical formula of the luminescent material is Zr1‑x‑y‑ zAxO2：yRE3+, zYb3+, wherein：0.03≤x≤0.5,0.003≤y≤0.15,0.005≤z≤0.15.To solve the problems such as oxidation zirconium base up-conversion luminescent material luminous intensity is not high and thing is mutually unstable, the present invention prepares presoma with chemical coprecipitation, after drying, grinding, 2~4h is calcined in 1100~1300 DEG C, obtains a series of zirconia solid solution base infrared up conversion luminescent powder materials.The material has that preparation technology is simple, and powder granule is small, thing mutually stablizes the features such as single, chemical stability is good, red green color is adjustable, luminous intensity is high, is had broad application prospects in biomolecular labeling, laser, infrared acquisition and the field such as false proof.
Description
Technical field：
The invention belongs to infrared up-conversion luminous material research field, is more precisely that one kind swashs in 980nm infrared lights
Give and send upper conversion powder body material of visible ray and preparation method thereof.
Background technology：
Up-conversion luminescence is that the emission process of short-wavelength light is produced under the exciting of long wavelength light.Up-conversion luminescent material exists
Short wavelength's all solid state laser, 3 D stereo are shown, optical fiber communication technology, biomarker, fiber amplifier, infrared detection technique
It is with a wide range of applications with the various fields such as false proof.
Up-conversion luminescent material is typically made up of matrix, activator and sensitizer three parts.At present, study it is more upper turn
Conversion materials activator has rare earth element er, Ho, Tm, Nd and Pr, and rare earth element y b is then a kind of very effective upwards converitng sensitization
Agent.Up-conversion luminescent material is broadly divided into fluorine (halogen) compound, oxide, oxyhalide and sulphur according to the difference of matrix components
Compound etc., fluorine (halogen) compound, which fastens transition material, has relatively low phonon energy, higher up-conversion luminescence efficiency, but it is made
Standby complex process, require high, heat endurance and chemical stability are poor.Same fluoride, testing sulphide ratio, oxide have simpler
Single preparation technology, more preferable heat endurance and chemical stability, can meet many-sided practical application.
Found by the literature search to prior art, the up-conversion luminescent material using oxide as matrix is studied in recent years
Ascendant trend is presented.Some Domestic, if Zhang Zhen crowd in 2009 et al. is being delivered Acta Optica《Er3+Adulterate TiO2Crystal structure
And its Upconversion luminescence》Mention and 0.1%~3.0% (molar fraction) Er is prepared for sol-gel process (sol-gel)3+
Dopen Nano TiO2Crystal；What Wang Jinxian in 2010 etc. was delivered《Gd2O3：Yb3+, Er3+The preparation of upper conversion nano fiber and table
Sign》Mention being combined with electrostatic spinning technique with sol-gel process and Gd is prepared2O3：Yb3+, Er3+Upper conversion nano fiber；
What Fan Yexia in 2011 et al. delivered in photon journal《Influence of the ytterbium concentration to the double-doped titanium dioxide up-conversion luminescence of holmium ytterbium》Carry
TiO is prepared for sol-gel process2：Ho3+/Yb3+Up-conversion luminescence nano-powder；What Zhai Xiang in 2013 et al. was delivered《ZnO：
The preparation of Er/Yb different-shape nano particles and up-conversion luminescence property research》In mention using the precipitation method, alkaline etching, mould
Plate method is prepared for the Zinc oxide doped rare earth element nano powder of different-shape.Foreign scholar is also to oxide as upper conversion material
Material matrix is studied：Such as《Visible upconversion emissions in Pr3+-doped TeO2-ZnO
glass》(Appl.Phys.B(2012)109：599-603)；Such as《Energy-Transfer-Up-conversion Models,
Their Applicability and Breakdown in the Presence of Spectroscopically
Distinct Ion Classes：A Case Study in Amorphous Al2O3：Er3+》(J.Phys.Chem.C
(2013), 117：6759-6776) etc., but the TiO selected in above-mentioned report2、ZnO、Gd2O3、TeO2-ZnO、Al2O3Deng oxide
The problems such as matrix generally existing phonon energy is higher, and upper conversion efficiency is relatively low.
ZrO2With wear-resistant, corrosion-resistant, high intensity, high-melting-point and good chemical stability and relatively low phonon energy
Measure (~470cm-1) the features such as, it is widely used in metallurgy, electronics, chemical industry, machinery, hair as structural material and functional material
The fields such as light.Chinese patent (publication number CN102660273A, CN102952543A, CN103045246A) is disclosed with oxygen in succession
Change different up-conversion luminescent materials of the zirconium as optical substrate, the luminescent properties of oxidation zirconium base up-conversion luminescent material are obvious good
It is that luminescent properties are preferable in oxide-base up-conversion luminescent material in up-conversion luminescent materials such as titanium oxide, zinc oxide, aluminum oxide
One kind, but its luminous intensity is not met by the needs of practical application, and zirconium oxide has three kinds of crystalline phase (m-ZrO2、t-ZrO2With
c-ZrO2), different its thing phase composition different with temperature in use of synthesis temperature are different.For example, the zirconium oxide of 800 DEG C of synthesis is monocline
Mutually with the mixed phase of cubic phase composition, the zirconium oxides of 1200 DEG C of synthesis are single monoclinic phase；There is phase between three kinds of crystalline phases
Transformation, be transformed into Tetragonal in 1170 DEG C or so monocline phase zircites, while with 5% or so bulk effect, occur compared with
Big stress, micro-crack even fragmentation can be produced in structure.The thing phase wild effect that this synthesis and temperature in use different band are come
The unstable of oxidation zirconium base up-conversion luminescent material performance is ultimately resulted in, limits its practical application.
The content of the invention：
For oxidation zirconium base up-conversion luminescent material luminous intensity is not high and the mutually unstable caused luminescent properties of thing not
The problems such as stable, the present invention with chemical coprecipitation be prepared for a kind of thing mutually stablize, the zirconia solid solution base that luminous intensity is high
The up-conversion luminescence powder material of matter.
To achieve these goals, technical scheme is as follows：
A kind of infrared up conversion luminescent powder materials chemistry formula disclosed by the invention is Zr1-x-y-zAxO2：yRE3+, zYb3+,
Wherein：Zr1-xAxO2To mix the zirconia solid solution matrix of elements A, 0.03≤x≤0.5, A are Sr and La, Gd, Lu, in Ce extremely
Few one kind, they play a part of stabilizing zirconia crystalline phase and improve up-conversion luminescence powder material emission intensity；Sr and La,
Gd, Lu, Ce play the role of stabilizing zirconia crystalline phase, and when A additions are few, Sr plays a major role, up-conversion luminescence powder material
For single tetragonal zircite structure, when A additions are more, La, Gd, Lu, Ce play a major role, and up-conversion luminescence powder material is
Single cubic oxide zircon-structure；RE3+For activator, 0.003≤y≤0.15, RE3+It is Er3+, Ho3+In one kind, mix Er3+
When, 0.003≤y≤0.15, mix Ho3+When, 0.003≤y≤0.02；Yb3+For sensitizer, 0.005≤z≤0.15.X, y, z point
The molar fraction of doped chemical A, activator and sensitizer is not represented.
The preparation method of infrared up conversion luminescent powder material of the present invention is made up of following steps：
(1) various rare earth nitre are conversed according to the content of each element in described infrared up conversion luminescent powder material composition
The dosage of hydrochlorate, basic zirconium chloride, it is the molten of 0.1~0.4mol/L to weigh and be made into cation concn with distilled water after various raw materials
Liquid, 10~30min of stirring make it well mixed, and polyethylene glycol PEG- is added into solution by solution and dispersant volume ratio 10: 1
400；
(2) 1~3molL is added-1Ammonia precipitation process agent, speed control is in 5~10mlmin-1, make pH value reach 9~
11, continue after 1~2h of stirring makes it fully react, to be aged 12~16h；
(3) filtered after removing supernatant liquid, with water washing is distilled 2~3 times, absolute ethyl alcohol washs 1~2 time, and filter cake exists
90~110 DEG C of dry 12~16h；
(4) will be calcined after dry product grinding, calcining heat is 1100~1300 DEG C, and the time is 2~4h, after calcining with
Stove cools down.
Compared with prior art, infrared up conversion luminescent powder material preparation process of the invention is simple, grain diameter is small,
Thing is mutually stable and single, heat endurance and chemical stability are good, and luminous intensity is high, can by adjust composition send it is green or red
Color visible ray, in short wavelength's all solid state laser, 3 D stereo show, biomolecular labeling, fiber amplifier, infrared acquisition skill
Art is with a wide range of applications with the field such as false proof.
Brief description of the drawings：
Fig. 1 is the infrared up conversion luminescent powder material Zr prepared using chemical coprecipitation0.925Sr0 03Ce0.03Er0.005Yb0.01O2XRD.
Fig. 2 is the infrared ray excited lower infrared up conversion luminescent powder materials of 980nm
Zr0.925Sr0.03Ce0.03Er0.005Yb0.01O2Up-conversion fluorescence spectrogram.
Fig. 3 is the infrared ray excited lower infrared up conversion luminescent powder material Zr of 980nm0.71Sr0.03Ce0.12Er0 11Yb0.03O2
Up-conversion fluorescence spectrogram.
Fig. 4 is the infrared ray excited lower up-conversion luminescence powder material Zr of 980nm0.925Sr0.03Ce0.03Er0.005Yb0.01O2With
Zr0 985Er0.005Yb0.01O2Up-conversion fluorescence comparison diagram.
Specific embodiment：
The present invention is further described through with reference to specific embodiment, but specific embodiment is not appointed to the present invention
What is limited.
Embodiment 1
Zr is prepared with chemical coprecipitation0.925Sr0.03Ce0.03Er0.005Yb0.01O2Infrared up conversion luminescent powder material, tool
Body is as follows：
A. 7.222g ZrOCl are weighed2·8H2O、0.154g Sr(NO3)3、0.317g Ce(NO3)3·6H2O、0.054g
Er(NO3)3·5H2O、0.113g Yb(NO3)3·6H2O is put into beaker, is added distilled water and is made into 200ml solution, and is added dropwise
20ml dispersant PEG-400, stir 10min；
B. solution 2mol/L ammoniacal liquor instilled in step A, speed control have white in 6ml/min or so, solution
Gelatinous precipitate generates, and works as pH=9, stops being added dropwise；
C. continue to be stirred vigorously 1h, after solution is fully reacted, close agitator, be aged 12h；
D. the supernatant liquid in beaker in step C is gone to filter, distillation water washing is used during suction filtration 3 times, then used
Absolute ethyl alcohol is washed 2 times, and filter cake is taken out and is put into beaker, is placed in electric heating bellows and is dried 12h, and temperature is set as 105 DEG C；
E. after the presoma dried object in D steps being taken out into cooling, it is put into agate mortar and is fully ground；
F. the sample in E steps is taken out and loads alumina crucible, be put into Muffle furnace and calcine, condition is set as：Heating
Speed is 5 DEG C/min, and 1200 DEG C are incubated 3h, furnace cooling.
From Fig. 1, we understand Zr0.925Sr0.03Ce0.03Er0.005Yb0.01O2Infrared up conversion luminescent powder material is by single
Tetragonal phase zirconium oxide solid solution crystalline phase form, illustrate in ZrO2Middle doping Sr and Ce serves stable ZrO2The effect of thing phase.Figure
2 be the up-conversion fluorescence spectrogram of the up-conversion luminescence powder material.980nm semiconductor laser of the powdered samples in 50mw
Under device irradiation, relatively bright green light is observed visually.
Embodiment 2
Zr is prepared with chemical coprecipitation0.71Sr0 03Ce0.12Er0.11Yb0.03O2Infrared up conversion luminescent powder material, tool
Body is as follows：
Weigh 5.543g ZrOCl2·8H2O、0.154g Sr(NO3)3、1.268g Ce(NO3)3·6H2O、1.187g Er
(NO3)3·5H2O、0.34g Yb(NO3)3·6H2O is put into beaker, is added distilled water and is made into 200ml solution, and is added dropwise
20ml dispersant PEG-400 stirrings 10min.
Remaining step is the same as embodiment 1.
At room temperature, Zr0 71Sr0.03Ce0.12Er0 11Yb0.03O2Infrared up conversion luminescent powder material is by single Emission in Cubic
Zirconia solid solution crystalline phase is formed.Fig. 3 is the up-conversion fluorescence spectrogram of the up-conversion luminescence powder material.The powdered samples
In 50mw 980nm semiconductor lasers irradiation, naked eyes are it is observed that bright bright-coloured red light.
Embodiment 3
Zr is prepared with chemical coprecipitation0.8Sr0.05La0 03Er0.01Yb0.11O2Infrared up conversion luminescent powder material, specifically
It is as follows：
Weigh 6.246g ZrOCl2·8H2O、0.256g Sr(NO3)3、0,315g La(NO3)3·6H2O、0.108g Er
(NO3)3·5H2O、1.245g Yb(NO3)3·6H2O is put into beaker, is added distilled water and is made into 200ml solution, and is added dropwise
20ml dispersant PEG-400 stirrings 10min；
Remaining step is the same as embodiment 1.
At room temperature, the powdered samples are observed visually stronger green in 50mw 980nm semiconductor lasers irradiation
Coloured light.
Embodiment 4
Zr is prepared with chemical coprecipitation0.79Sr0.05La0.05Er0.09Yb0.07O2Infrared up conversion luminescent powder material, tool
Body is as follows：
Weigh 6.168g ZrOCl2·8H2O、0.256g Sr(NO3)3、0.525g La(NO3)3·6H2O、0.971g Er
(NO3)3·5H2O、0.792g Yb(NO3)3·6H2O is put into beaker, is added distilled water and is made into 200ml solution, and is added dropwise
20ml dispersant PEG-400 stirrings 10min；
Remaining step is the same as embodiment 1.
At room temperature, for the powdered samples in 50mw 980nm semiconductor lasers irradiation, naked eyes are it is observed that pure
Red light.
Embodiment 5
Zr is prepared with chemical coprecipitation0.805Sr0.07Gd0.05Ho0.005Yb0.07O2Infrared up conversion luminescent powder material, tool
Body is as follows：
Weigh 6.285g ZrOCl2·8H2O、0.359g Sr(NO3)3、0.547g Gd(NO3)3·6H2O、0.057g Ho
(NO3)3·5H2O、0.792g Yb(NO3)3·6H2O is put into beaker, is added distilled water and is made into 200ml solution, and is added dropwise
20ml dispersant PEG-400 stirrings 10min；
Remaining step is the same as embodiment 1.
At room temperature, the powdered samples are in 50mw 980nm semiconductor lasers irradiation, and naked eyes are it is observed that bright
Green light.
Embodiment 6
Zr is prepared with chemical coprecipitation0.735Sr0.07Gd0.1Ho0.005Yb0 09O2Infrared up conversion luminescent powder material, tool
Body is as follows：
Weigh 5.738g ZrOCl2·8H2O、0.359g Sr(NO3)3、1.094g Gd(NO3)3·6H2O、0.057g Ho
(NO3)3·5H2O、1.019g Yb(NO3)3·6H2O is put into beaker, is added distilled water and is made into 200ml solution, and is added dropwise
20ml dispersant PEG-400 stirrings 10min；
Remaining step is the same as embodiment 1.
At room temperature, the powdered samples are in 50mw 980nm semiconductor lasers irradiation, and naked eyes are it is observed that bright
Green light.
Comparative example 1
Zr is prepared with chemical coprecipitation0.985Er0.005Yb0.01O2Infrared up conversion luminescent powder material, it is specific as follows：
As the comparative example with embodiment 1, this example weighs 7.690g ZrOCl2·8H2O、0.054g Er(NO3)3·
5H2O、0.113g Yb(NO3)3·6H2O is put into beaker, is added distilled water and is made into 200ml solution, and 20ml point is added dropwise
Powder PEG-400 stirs 10min；
Remaining step is the same as embodiment 1.
At room temperature, the powdered samples 50mw 980nm semiconductor lasers irradiation when, be observed visually its send compared with
Weak green glow.And the Zr of the present invention0.925Sr0.03Ce0.03Er0 005Yb0.01O2Infrared up conversion luminescent powder material is in similarity condition
Under send relatively bright green glow.It can be seen that from accompanying drawing 4：It is infrared in the case of identical activator and sensitizer incorporation
The matrix composition of up-conversion luminescence powder material influences very big, Zr to the luminescent properties of material0.985Er0.005Yb0.01O2Zirconium oxide
Luminous weaker, the Zr of the present invention of base up-conversion luminescence powder material0.925Sr0.03Ce0.03Er0.005Yb0.01O2Zirconium oxide
The luminous intensity of solid solution base up-conversion luminescence powder material is significantly higher than Zr0.985Er0.005Yb0.01O2Aoxidize and hair is changed in zirconium base
The luminous intensity of light powder body material.
Claims (10)
- A kind of 1. zirconia solid solution base infrared up conversion luminescent powder material and preparation method thereof, it is characterised in that useization Learn coprecipitation and prepare the infrared up conversion luminescent powder material that zirconia solid solution is matrix, its chemical formula is：Zr1-x-y- zAxO2：yRE3+, zYb3+, wherein, Zr1-xAxO2For matrix, RE3+For activator, Yb3+For sensitizer, x, y, z represents doping respectively Elements A, activator RE3+With sensitizer Yb3+Molar fraction.
- 2. infrared up conversion luminescent powder material according to claim 1, it is characterised in that the base of the up-conversion Matter is to mix the zirconia solid solution of elements A, and A is Sr and La, Gd, Lu, at least one of Ce.
- 3. infrared up conversion luminescent powder material according to claim 1, it is characterised in that the up-conversion conduct Activator is rare earth ion Er3+, Ho3+In one kind.
- 4. infrared up conversion luminescent powder material according to claim 1, it is characterised in that the up-conversion conduct Sensitizer is rare earth ion Yb3+。
- 5. infrared up conversion luminescent powder material according to claim 1 or 2, it is characterised in that doping element A x takes Value scope is：0.03≤x≤0.5.
- 6. the infrared up conversion luminescent powder material according to claim 1 or 3, it is characterised in that activator RE3+Y take Value scope is：0.003≤y≤0.15.
- 7. the infrared up conversion luminescent powder material according to claim 1 or 4, it is characterised in that sensitizer Yb3+Z take Value scope is：0.005≤z≤0.15.
- 8. the preparation method of infrared up conversion luminescent powder material according to claim 1, it is characterised in that made with ammoniacal liquor For the chemical coprecipitation of precipitating reagent.
- 9. the preparation of infrared up conversion powder body material according to claim 1, it is characterised in that specifically include following step Suddenly：(1) content of each element converses the dosage of various rare earth nitrades, basic zirconium chloride in being formed according to material, weighs various The solution that cation concn is 0.1~0.4mol/L is made into distilled water after raw material, 10~30min of stirring makes it well mixed, Polyethylene glycol PEG-400 is added into solution by solution and dispersant volume ratio 10: 1；(2) 1~3molL is added-1Ammonia precipitation process agent, speed control is in 5~10mlmin-1, pH value is reached 9~11；(3) after continuing 1~2h of stirring and it is fully reacted, it is aged 12~16h；(4) filtered after removing supernatant liquid, with distillation water washing 2~3 times, absolute ethyl alcohol washs 1~2 time, filter cake 90~ 110 DEG C of dry 12~16h；(5) will be calcined after dry precursor product grinding, calcining heat is 1100~1300 DEG C, and the time is 2~4h, after calcining Furnace cooling.
- 10. the preparation method according to claim 1 or 9, it is characterised in that in step (5), calcining heat be 1100~ 1300 DEG C, the time is 2~4h.
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Application publication date: 20180112 |