CN1687306A - Luminescent material converted in nano level with yttrium oxide as matrix and preparation method - Google Patents
Luminescent material converted in nano level with yttrium oxide as matrix and preparation method Download PDFInfo
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- CN1687306A CN1687306A CN 200510025618 CN200510025618A CN1687306A CN 1687306 A CN1687306 A CN 1687306A CN 200510025618 CN200510025618 CN 200510025618 CN 200510025618 A CN200510025618 A CN 200510025618A CN 1687306 A CN1687306 A CN 1687306A
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Abstract
The present invention relates to a rare earth ion double-doped or three-doped or three-doped yttrium oxide base up-conversion luminescence material and its preparation method. It is characterized by that said invention adopts coprecipitation process to dope two kinds or three kinds of rare earth ions into yttrium oxide matrix so as to implement high-effective up-conversion luminescence. The grain size of yttrium raise base up-conversion luminescence powder obtained by said invention is 60-80 nm, under the excitation of infrared radiation with 808 or 980 nm wavelength it can implement up-conversion luminescence of several different colour of blue, green, red and orange. Besides, said invention also provides its application range.
Description
Technical field
The present invention relates to a kind of rare earth ion doped yttria-base up-conversion luminescent material and preparation method thereof, more precisely relating to a kind of is the rare earth ion codope of matrix or three adulterated luminescent material converted in nano level and preparation method thereof with the yttrium oxide, belongs to luminescent material and preparation technology field thereof in the shiner Neo-Confucianism.
Background technology
Up-conversion luminescent material is that a kind of ir radiation the long wavelength excites the material of launching short wavelength's visible light down, it is at (the Zarling that is with a wide range of applications such as 3 D stereo demonstration, short wavelength's all solid state laser, biomolecules fluorescent mark, infrared detective, aspect such as false proof, et al., USpatent 5674698,1997).
The higher up-conversion of efficient mainly is various rare earth ion doped halogenide, the glass or the monocrystalline of oxyhalogenide at present, this mainly is because these materials have lower phonon energy, low matrix phonon energy, can suppress the probability of radiationless transition, thereby obtain higher up-conversion luminescence efficient.Yet the chemical stability of these materials is generally relatively poor, and the preparation difficulty, needs special equipment and condition.These shortcomings have seriously hindered up-conversion and have moved towards practical application.Yttrium oxide has better chemical and photochemical stability, and the thermal conductivity height, is easy to realize the high-concentration dopant of rare earth ion, and these advantages make it become a kind of good luminescent material matrix (solid luminescence, Jilin physics Suo ﹠amp; China Science ﹠ Technology University, 1976, p57-p60).In fact, Y
2O
3: Eu
3+Red fluorescence powder material as a kind of excellent performance, be widely used in photoluminescence already, field (JunyingZhang such as cathodoluminescence and X ray are luminous, Zhongtai Zhang, Zilong Tang, Yuanhua Lin, Zishang Zheng, " luminescentproperties of Y
2O
3: Eu synthesized by sol-gel processing, Journal of MaterialProcessing Technology, 121 (2002) 265-268).Studies show that yttrium oxide also has lower phonon energy, its phonon energy is 430-550cm
-1(L.A.Riseberg, " The Relevance ofNonradiative Transitions to Solid State Lasers " pp.369-407 in NATO AdvancedStudy Institute Series, Series B:Physics, Vol.62, Radiationless Processes Editedby B.DiBartolo.Plenum Press, New York, 1980), this is suitable with the phonon energy of going up the higher ZBLAN material of efficiency of conversion at present.Therefore, by selecting the concentration of suitable dopant ion, co-dopant ions and dopant ion, can in this system, obtain to go up efficiently switching emission fully.
Summary of the invention
The objective of the invention is to propose a kind of is the rare earth ion codope of matrix or three adulterated up-conversion luminescent materials and preparation method thereof with the yttrium oxide, this method technology is simple, do not need special equipment, the diameter of particle that is obtained is about 60nm, even particle distribution, infrared upward efficiency of conversion height, stable performance, can be entrained in the different material of multiple physical and chemical performance, be used for fields such as infrared detective, false proof and biomolecules fluorescent mark.
A kind of rare earth ion doped be the luminescent material converted in nano level of matrix with the yttrium oxide, it is characterized in that: it is to be matrix with the yttrium oxide, and the concentration of the oxide compound of doped with rare-earth elements Yb or Nd is that the concentration of the oxide compound of 1～30mol%, doped with rare-earth elements Er, Tm, Ho, Tb, Pr, Eu, Dy, Sm is 0.1%～15mol%.The up-conversion luminescent material particle diameter 60-80nm that is provided, and be single cubic structure.
Provided by the present invention rare earth ion doped be that the luminescent material converted in nano level of matrix adopts coprecipitation method preparation technology with the yttrium oxide, main raw material is Y
2O
3, Yb
2O
3, Nd
2O
3, Ho
2O
3, Er
2O
3, Tm
2O
3, Sm
2O
3, Tb
4O
7, Pr
6O
11, Eu
2O
3, Dy
2O
3, Sm
2O
3, the purity of rare earth oxide＞99.99%, bicarbonate of ammonia (analytical pure), ammoniacal liquor (analytical pure), hydrochloric acid (analytical pure), nitric acid (analytical pure), ethanol (chemical pure).The present invention implements by following technological process:
1, the preparation of rare earths salt: with rare earth oxide Y
2O
3, Yb
2O
3, Nd
2O
3, Ho
2O
3, Er
2O
3, Tm
2O
3, Sm
2O
3, Tb
4O
7, Pr
6O
11, Eu
2O
3, Dy
2O
3, Sm
2O
3Be dissolved in hydrochloric acid or the nitric acid, being diluted to oxide content concentration is 10g/l-80g/l, and adjusting pH value is 2～4.
2, the preparation of precipitant solution: ammoniacal liquor or bicarbonate of ammonia is dissolved in is mixed with solution in the deionized water, the concentration of control ammoniacal liquor is 0.5～5mol/l, and the concentration of ammonium hydrogencarbonate is 0.5～3mol/l.
3, powder preparing: precipitant solution speed with 1～10ml/min under intense stirring condition is added drop-wise in the mixing solutions of rare-earth salts, obtain gelatinous precipitate, or employing back titration method, rare earth nitrate or muriate mixing solutions are titrated in ammoniacal liquor or the ammonium bicarbonate soln, obtain gelatinous precipitate; Titration speed also is 1-10ml/min.Treat to continue to stir 0.5～2h, still aging 15～48h under the room temperature then again after the titration fully.With 5～10 flush away NH of deionized water wash
4NO
3Perhaps NH
4Cl, with 3～5 dehydrations of absolute ethanol washing, suction filtration obtains filter cake then again.Filter cake is placed in the baking oven 60 ℃～120 ℃ drying 8～24h under air conditions.Powder after the final drying is warming up to 750 ℃～950 ℃ and be incubated 2-4h with the speed of 3～8 ℃/min, then furnace cooling under air conditions.
The invention provides a kind of rare earth ion doped yttria-base up-conversion luminescent material and preparation method thereof, have the following advantages:
Yttria-base up-conversion luminescent material provided by the present invention adopts rare earth ion codope or three doped forms, has higher last efficiency of conversion, and the more traditional fluorochemical of chemical property is stablized, this powder can be entrained in the different material of multiple physical and chemical performance, is used for fields such as infrared detective, false proof and biomolecules fluorescent mark;
By selecting different doping with rare-earth ions, codoped rare earth ion and different dopant ion concentration, 808 or the ir radiation of 980nm wavelength excite down, the yttria-base up-conversion luminescent material can be realized the up-conversion luminescence of blueness, green, redness, yellow multiple different colours;
Owing to adopted coprecipitation technology to prepare rare earth ion doped yttrium oxide powder, can guarantee the even doping of rare earth ion, the diameter of particle that obtains is evenly distributed, granular size is 60-80nm, be nanometer grade powder, and preparation technology is simple, need not specific installation, be convenient to scale operation.The powder that is provided can be entrained in the different material of multiple physical and chemical performance, is used for fields such as infrared detective, false proof and biomolecules fluorescent mark.
Description of drawings
Fig. 1 analyzes (wherein: a is pure yttrium oxide, and b contains rare earth ion doped yttrium oxide) for the XRD crystalline phase of the sample after calcining.Diffraction peak among the figure does not have other dephasigns to occur all corresponding to the cubic oxide yttrium, shows that the complete solid solution of rare earth ion is in Y
2O
3Lattice.
Fig. 2 is the field emission scanning electron microscope photo after sample is calcined through 850 ℃/2h.As seen from the figure, the even particle distribution of powder, particle size is about 60nm.
Fig. 3 is embodiment 1 described Yb
2O
3And Er
2O
3The codope yttrium oxide powder emission wavelength be under the semiconductor laser of 980nm excites on inversion spectrum.
Fig. 4 is embodiment 4 described Yb
2O
3And Ho
2O
3The codope yttrium oxide powder emission wavelength be under the semiconductor laser of 980nm excites on inversion spectrum.
Fig. 5 is embodiment 5 described Yb
2O
3And Tm
2O
3The codope yttrium oxide powder emission wavelength be under the semiconductor laser of 980nm excites on inversion spectrum.
Embodiment
Embodiment 1
With 22.58 gram Y
2O
3, 0.42 the gram Yb
2O
3, 0.04 the gram Er
2O
3Be dissolved in the nitric acid, add deionized water and be diluted to 1L, regulating its pH value with ammoniacal liquor is 2～3, and stirs.The 60ml strong aqua is dissolved in the deionized water, be made into the ammonia soln 450ml of 2mol/l, after mixing, under intense stirring condition, speed with 10ml/min is added drop-wise in the mixture solution of rare earth ion, obtain gelatinous precipitate, treat to continue to stir 2h, still aging 24h under the room temperature then again after the titration fully.With deionized water wash 5 times, with flush away NH
4NO
3After, using absolute ethanol washing again 4 times, 80 ℃ of dry 24h under the air conditions in baking oven at last are put in the alumina crucible 850 ℃ of calcining 2h in retort furnace with dried presoma, obtain Y
2O
3: Yb
3+, Er
3+Green up-conversion luminescence powder.This diameter of particle is about 60nm, and even particle distribution is single cubic structure (as shown in Figure 1, 2), is that the semiconductor laser of 808nm or 980nm excites and launches bright green up-conversion fluorescence down at wavelength.As shown in Figure 3, for sample wavelength be under the semiconductor laser of 980nm excites on inversion spectrum, two main emission bands of green glow and ruddiness are arranged among the figure, peak emission wavelength is positioned at 562nm and 660nm, corresponds respectively to Er
3+Ionic
4S
3/2/
2H
11/2→
4I
15/2With
4F
9/2→
4I
15/2Energy level transition.
Embodiment 2
With 22.58 gram Y
2O
3, 8.44 the gram Yb
2O
3, 8.20 the gram Er
2O
3Be dissolved in the hydrochloric acid, add deionized water and be diluted to 1L, regulating its pH value with ammoniacal liquor is 2～3, and mixes.32.94g bicarbonate of ammonia is dissolved in the deionized water, be made into the ammonium bicarbonate soln 417ml of 1mol/l, after mixing, under intense stirring condition, speed with 5ml/min is added drop-wise in the mixture solution of rare earth ion, obtain gelatinous precipitate, treat to continue to stir 2h, still aging 36h under the room temperature then again after the titration fully.Wash NH off 7 times with deionized water wash
4Behind the Cl, use absolute ethanol washing again 4 times, 80 ℃ of dry 24h under the air conditions in baking oven at last are put in the alumina crucible 850 ℃ of calcining 2h in retort furnace with dried precipitation, obtain Y
2O
3: Yb
3+, Er
3+Orange-yellow up-conversion luminescence powder.This diameter of particle is about 60nm, and even particle distribution is single cubic structure (as shown in Figure 1, 2), is that the semiconductor laser of 808nm or 980nm excites and launches bright orange-yellow up-conversion fluorescence down at wavelength.
Embodiment 3
With 22.58 gram Y
2O
3, 1.66 the gram Yb
2O
3, 0.40 the gram Er
2O
3Be dissolved in the nitric acid, add deionized water and be diluted to 1L, regulating its pH value with ammoniacal liquor is 2～3, and mixes.The 60ml strong aqua is dissolved in the deionized water, be made into the ammonia soln 450ml of 2mol/l, under intense stirring condition, speed with 10ml/min is added drop-wise in the mixture solution of rare earth ion, obtain the gelatinous precipitate of white, treat to continue to stir 2h, still aging 24h under the room temperature then again after the titration fully.Wash NH off 5 times with deionized water wash
4NO
3After, using absolute ethanol washing again 4 times, 100 ℃ of dry 8h under the air conditions in baking oven at last are put in the alumina crucible 750 ℃ of calcining 4h in retort furnace with dried precipitation, obtain Y
2O
3: Yb
3+, Er
3+Red up-conversion luminescence powder.This diameter of particle is about 60nm, and even particle distribution is single cubic structure.At wavelength is that the semiconductor laser of 808nm or 980nm excites and launches bright red up-conversion fluorescence down.
Embodiment 4
With 22.58 gram Y
2O
3, 1.44 the gram Yb
2O
3, 0.18 the gram Ho
2O
3Be dissolved in the nitric acid, add deionized water and be diluted to 1L, regulating its pH value with ammoniacal liquor is 2～3, and mixes.The 60ml strong aqua is dissolved in the deionized water, be made into the ammonia soln 450ml of 2mol/l, under intense stirring condition, speed with 10ml/min is added drop-wise in the mixture solution of rare earth ion, obtain the gelatinous precipitate of white, treat to continue to stir 2h, still aging 48h under the room temperature then again after the titration fully.Wash NH off 7 times with deionized water wash
4Behind the CL, use absolute ethanol washing again 4 times, 80 ℃ of dry 24h under the air conditions in baking oven at last are put in the alumina crucible 950 ℃ of calcining 2h in retort furnace with dried precipitation, obtain Y
2O
3: Yb
3+, Ho
3+The up-conversion luminescence powder.This diameter of particle is about 80nm, and even particle distribution is single cubic structure.At wavelength is that the semiconductor laser of 980nm excites down and launches bright green up-conversion fluorescence, as shown in Figure 4.Mainly contain green glow, two main emission bands of ruddiness among the figure, peak emission wavelength is positioned at 549m and 666nm, corresponds respectively to Ho
3+Ionic
5S
2/
5F
4→
5I
8With
5F
5→
5I
8Energy level transition; In addition, can also observe the near infrared emission that peak value is positioned at 755nm, derive from Ho
3+Ionic
5S
2/
5F
4→
5I
7Energy level transition.
Embodiment 5
With 22.58 gram Y
2O
3, 1.44 gram Yb
2O
3, 0.20 the gram Tm
2O
3Be dissolved in the hydrochloric acid, add deionized water and be diluted to 1L, regulating its pH value with ammoniacal liquor is 2～3, and mixes.32.94g bicarbonate of ammonia is dissolved in the deionized water, be made into the ammonium bicarbonate soln 417ml of 1mol/l, under intense stirring condition, speed with 10ml/min is added drop-wise in the mixture solution of rare earth ion, obtain gelatinous precipitate, treat to continue to stir 2h, still aging 24h under the room temperature then again after the titration fully.Wash NH off 7 times with deionized water wash
4Behind the Cl, use absolute ethanol washing again 4 times, 80 ℃ of dry 24h under the air conditions in baking oven at last are put in the alumina crucible 850 ℃ of calcining 2h in retort furnace with dried precipitation, obtain Y
2O
3: Yb
3+, Tm
3+Blue up-conversion luminous powder.This diameter of particle is about 60nm, and even particle distribution is single cubic structure.At wavelength is that the semiconductor laser of 808nm excites down and launches bright blue up-conversion fluorescence, and naked eyes are high-visible, as shown in Figure 5.Two main emission bands of blue light and ruddiness are arranged among the figure, and peak emission wavelength is positioned at 486nm and 652nm, corresponds respectively to Tm
3+Ionic
1G
4→
3H
6With
1G
4→
3F
4Energy level transition.
Embodiment 6
With 22.58 gram Y
2O
3, 4.05 gram Nd
2O
3, 2.37 the gram Yb
2O
3, 0.92 the gram Er
2O
3Be dissolved in the hydrochloric acid, add deionized water and be diluted to 1L, regulating its pH value with ammoniacal liquor is 2～3, and mixes.32.94g bicarbonate of ammonia is dissolved in the deionized water, be made into the ammonium bicarbonate soln 417ml of 1mol/l, under intense stirring condition, speed with 10ml/min is added drop-wise in the mixture solution of rare earth ion, obtain gelatinous precipitate, or use the back titration mode, the muriate mixing solutions of above-mentioned rare earth oxide is added drop-wise to obtains gluey coprecipitate in the ammonium bicarbonate soln.Treat to continue to stir 2h, still aging 15h under the room temperature then again after the titration fully.Wash NH off 7 times with deionized water wash
4Behind the Cl, use absolute ethanol washing again 4 times, 80 ℃ of dry 24h under the air conditions in baking oven at last are put in the alumina crucible 850 ℃ of calcining 2h in retort furnace with dried precipitation, obtain Y
2O
3: Nd
3+, Yb
3+, Er
3+Three adulterated green up-conversion luminescence powders.This diameter of particle is about 60nm, and even particle distribution is single cubic structure.Wavelength be 808 or the semiconductor laser of 980nm excite down and launch bright green up-conversion fluorescence, naked eyes are high-visible.
Claims (9)
1, a kind of is the luminescent material converted in nano level of matrix with the yttrium oxide, is doped element with the rare earth ion, it is characterized in that the Doped Rare Earth element is two kinds or three kinds among Yb, Nd, Er, Tm, Ho, Tb, Pr, Eu, Dy or the Sm; The concentration of the oxide compound of doped with rare-earth elements Yb or Nd is that the concentration of the oxide compound of 1～30mol%, doped with rare-earth elements Er, Tm, Ho, Tb, Pr, Eu, Dy, Sm is 0.1%～15mol%.
2, according to claim 1 is the luminescent material converted in nano level of matrix with the yttrium oxide, it is characterized in that described luminescent material converted in nano level particle diameter 60-80nm, and is single cubic structure.
3, preparation is as claimed in claim 1 is the method for the luminescent material converted in nano level of matrix with the yttrium oxide, it is characterized in that comprising following concrete steps:
(1) adopting rare earth oxide is starting raw material, is dissolved in nitric acid or the hydrochloric acid, is mixed with rare earth nitrate or muriate mixing solutions, and rare earth oxide content is 10-80g/l; The pH value of regulator solution is 2～4;
(2) be added drop-wise in the mixture solution of the rare earth ion that step (1) makes with the speed of 1～10ml/min under intense stirring condition with ammoniacal liquor or ammonium bicarbonate soln, obtain gluey coprecipitate, through stirring, ageing, deionized water flush away NH wherein
4NO
3Perhaps NH
4The Cl after-filtration then with absolute ethanol washing, makes it to be converted into oxide powder through super-dry, calcining; Calcining temperature is 750-950 ℃.
4, as claimed in claim 3 is the preparation method of the luminescent material converted in nano level of matrix with the yttrium oxide, it is characterized in that the described coprecipitation method of step (2), or employing back titration method, rare earth nitrate or muriate mixing solutions are titrated in ammoniacal liquor or the ammonium bicarbonate soln, thereby obtain the co-precipitation powder; Titrating speed is 1-10ml/min.
5, described by claim 3 is the preparation method of the luminescent material converted in nano level of matrix with the yttrium oxide, it is characterized in that the concentration of precipitation agent ammoniacal liquor or bicarbonate of ammonia is respectively 0.5-5.0mol/l and 0.5-3.0mol/l.
6, by claim 3 or 4 described be the preparation method of the luminescent material converted in nano level of matrix with the yttrium oxide, the concentration that it is characterized in that the mixing solutions of described rare earth nitrate or rare earth chloride is 0.05-1.0mol/l.
7, by claim 3 or 4 described be the preparation method of the luminescent material converted in nano level of matrix with the yttrium oxide, it is characterized in that continuing to stir 0.5-2h behind the gluey coprecipitate of gained after the titration, ageing 15-48hr under the room temperature then, and with 5-10 washing of deionized water; Remove NH
4NO
3Or NH
4Cl uses absolute ethanol washing 3-5 time again, and suction filtration was at 60-120 ℃ of dry 8-24 hour.
8, by claim 3 or 4 described be the preparation method of the luminescent material converted in nano level of matrix with the yttrium oxide, temperature rise rate 3-8 ℃/min when it is characterized in that calcining is incubated 2-4 hour.
9, by claim 1 or 2 described be the preparation method of the luminescent material converted in nano level of matrix with the yttrium oxide, it is characterized in that different according to institute's doping with rare-earth ions and doping content, 808 or the ir radiation of 980nm wavelength excite down, thereby realize up-conversion luminescence blue, green, red, yellow multiple different colours.
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