CN102504818A - Method for preparing Ce3+-doped Lu3Al5Ol2 (lutetium aluminate) polycrystalline luminescent film - Google Patents
Method for preparing Ce3+-doped Lu3Al5Ol2 (lutetium aluminate) polycrystalline luminescent film Download PDFInfo
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Abstract
The invention relates to a method for preparing Ce3+-doped Lu3Al5Ol2 (lutetium aluminate) polycrystalline luminescent film, which belongs to the technical field of preparation technology of rare-earth compound luminescent films. The method is characterized by using lutetium chloride, aluminum nitrate, cerous nitrate and absolute ethyl alcohol as raw materials, using citric acid as complexing agent and polyethylene glycol as crosslinking agent, and using Pechini sol-gel process and spin coating process to prepare the Ce3+ ion doped LuAG polycrystalline luminescent film. The method has the advantages that synthesis temperature is low, doping is uniform, equipment cost is low, preparation processes are simple, the surface of the prepared film is smooth and crackless, and the film has good microstructure and optical properties.
Description
Technical field
The present invention relates to a kind of Ce
3+Adulterated Lu
3Al
5O
12(LuAG) preparation method of polycrystalline light emitting film belongs to rare earth compound light-emitting film fabricating technology field.
Background technology
The develop rapidly of Along with computer technology, digital imaging system such as X ray computer-tomography are because the advantage of fast imaging begins to move towards stage.The XCT imaging technique can deserve to be called the revolution of x-ray imaging, and this digital x-ray imaging system plays an important role at aspects such as medical treatment, industry, safety checks.Its center used scintillator of probe mainly contains scintillation crystals such as CsI (Tl), BGO, CdWO4.Though advantages such as this digital imaging system has conveniently, detection in real time,, its resolving power is generally in hundreds of micron ~ 1 a millimeter magnitude.
To the problem that improves resolving power, proposition such as Andreas Koch in 1998 are used than heavy material growing film scintillation material improving the idea of x ray absorption capacity and its resolving power of raising, and utilize liquid phase epitaxial method at the thick Y of 5um
3Al
5O
12Growth E u and the adulterated Lu of Tb on the substrate
3Al
5O
12The film scintillation material, film thickness can reach 1～100um, has successfully obtained the blind spider knee faultage image that resolving power is about 2um.Therefore, have nano level more the research of high spatial resolution flicker film receive much concern.
The flicker film is compared with the image display that luminescent powder is processed, and the tack of homogeneity, density, substrate all demonstrates stronger meliority, and the flicker film can effectively improve imaging resolution to light scattering hardly.Compare with scintillator crystal materials, preparation film scintillator desired equipment is comparatively simple, can large area deposition, be convenient to processing.Especially for multi-component material, can reach submicron even molecular level level with adulterated ion distribution in the film of chemical process (like sol-gel method) preparation.The flicker film plays an important role in fields such as medical science and biology as the important component part of imaging system.
Lu
3Al
5O
12Has cubic crystal structure (isometric system, spacer Ia3d), high (6.73 g/cm of density
3, be that present PET goes up material therefor Bi
4Ge
3O
12(BGO) 94%), fusing point high (2010 ℃), good mechanical property can be a kind of good flicker substrate material at long-term radiation condition stable optics and the physical and chemical performance of maintenance down.Because Ce
3+The 5d that allows
The 4f transition makes its quick fall time with tens nanoseconds, and the emission wavelength about 500～550 nm is satisfied with the scintillator performance requriements in the scope of the high sensitizing range of Si photorectifier, is a kind of very promising scintillation material.So Ce
3+Doping aluminic acid lutetium film has the photoyield height, and fall time is short and twilight sunset is little, and to the uptake factor big (high-density and big effective atomic number) of x ray, advantages such as emission wavelength and existing detecting element coupling are a kind of scintillator materials of very potentialization.
At present, some reports have been arranged, have mainly concentrated on powder, pottery, monocrystalline and monocrystal thin films aspect about the research of cerium ion-doped aluminic acid lutetium material, and the research of polycrystal film also do not appear in the newspapers to.Lu
3Al
5O
12Monocrystal material adopt Czochralski method growth usually, the complicated process of preparation of this method is harsh, cost is high, rare earth ion doped homogeneity is difficult to control, and the monocrystalline of very difficult growing large-size.2007, people such as Yu. Zorenko utilized liquid phase epitaxial method (PLE) to prepare Lu
3Al
5O
12: Ce (LuAG:Ce) monocrystal thin films used the same method on the YAG substrate afterwards and had prepared R
3Al
5O
12(R=Lu, Yb, Tb; Eu – Y) monocrystal thin films, 2009, people such as V. Gorbenko utilized liquid phase epitaxial method on the YAG substrate, to prepare LuAG:Pr and YAG:Pr monocrystal thin films; 2010; Seminars such as Jiri A. Mares and M Kucera utilize liquid phase epitaxial method (PLE) method to prepare cerium ion-doped LuAG film, but its growth temperature of this method is higher, dopant ion skewness and exist the problem etc. of monocrystal thin films and substrate lattice mismatch all to influence the quality of film all the time; It is restricted in practical application, and this preparation method not only cost height and complex process.With respect to additive method, advantage such as Pechini Rong Jiao – gel method has that synthesis temperature is low, uniform doping, equipment price are low.Meaning of the present invention is to utilize the Pechini sol-gel method to prepare the polycrystal film of the cerium ion-doped aluminic acid lutetium of excellent property.
Summary of the invention
The object of the present invention is to provide a kind of Pechini sol-gel method to combine spin coating proceeding to prepare Ce
3+The preparation method of the aluminic acid lutetium polycrystalline light emitting film of ion doping.
The present invention is a raw material with lutecium chloride, absolute ethyl alcohol, aluminum nitrate, cerous nitrate mainly; Be complexing agent with the Hydrocerol A, be linking agent, adopt the Pechini sol-gel method to combine spin coating proceeding and calcining process to prepare the Ce of good dispersivity, smooth surface, flawless, good luminous performance with polyoxyethylene glycol (PEG)
3+The aluminic acid lutetium polycrystalline light emitting film of ion doping.
The present invention is a kind of Ce
3+The preparation method of the aluminic acid lutetium polycrystalline light emitting film of ion doping is characterized in that following preparation process and step:
(a), the preparation of colloidal sol: according to chemical formula Lu
3 (1-X)Al
5O
12: xCe, x are x, and each element chemistry metering ratio in the chemical formula is pressed in x=0.002～0.01, takes by weighing a certain amount of LuCl
36H
2O (99.99%) powder joins in the 5ml deionized water; Ce (the NO that adds an amount of aluminum nitrate and 0.522mol/L again
3)
3Solution; Under 80 ° of C temperature, stir and made powder dissolve acquisition water white transparency shape solution fully in 1.5 hours; In gained solution, add polyoxyethylene glycol and the Hydrocerol A of an amount of 40mg/ml afterwards, the quality of Hydrocerol A is n with the ratio of the quality of total metals ion
Hydrocerol A: n
Metals ion=2:1; Add aqueous ethanolic solution again, the volume ratio of ethanol and water is V
C2H5OH: V
H2O=8:1; At room temperature stirred 1.5 hours, and promptly obtained required precursor colloidal sol;
(b), the cleaning of silicon substrate: earlier with the zone of oxidation of hydrofluoric acid rinsing 10min with the removal silicon face; Prevent that ionic from staining again; Next successively with acetone, ethanol, water ultrasonic cleaning 20min impurity such as particle with the removal silicon face; Use the vitriol oil and SPA mixing solutions (volume ratio is 3:1) to soak 24h to remove the harmful metal ion of silicon face at last, the monocrystalline silicon piece after the immersion is distinguished water and absolute ethyl alcohol ultrasonic cleaning 10min before use again to remove the residual acid solution of silicon face;
(c), spin coating and thermal pretreatment: the monocrystalline silicon piece that cleans up is flat on the microscope carrier of sol evenning machine, drips 3-4 to the even colloid that leaves standstill with dropper and drip to silicon face, the rotating speed of regulating sol evenning machine is coated on the silicon substrate colloid equably.The substrate of colloidal sol in the spin coating is transferred to roasting glue machine thermal treatment 5 min under 110 ° of C,, transfers to low temperature oven and heat-treat, remove organism such as surperficial polyoxyethylene glycol and Hydrocerol A to remove surface adsorption water and ethanol.Repetitive operation coating procedure several times obtain the film of desired thickness;
(d), calcining: will place retort furnace through the precursor thin-film that above-mentioned steps obtains, 800～1100
oThe C temperature lower calcination is handled, and is incubated 1-10 hour, and naturally cooling in air finally obtains even, transparent, flawless Ce then
3+Adulterated LuAG:Ce
3+Film.
Description of drawings
Fig. 1 is that the XRD figure of the film sample behind the calcining 2h under the differing temps reaches and the PDF card of standard aluminic acid lutetium contrasts.
Fig. 2 is exciting and emmission spectrum figure of calcination 2h obtains under 1000 ℃ of temperature film sample.
Fig. 3 is the Lu of the various ce doping content that calcination 2h obtains under 1000 ℃ of temperature
3 (1-X)Al
5O
12: the emmission spectrum figure of xCe (x=0.002,0.005,0.008,0.01) film.
Fig. 4 is the AFM figure of the film sample that calcination 2h obtains under 1000 ℃ of temperature.(a) plat, (b) three-dimensional plot.
Fig. 5 is the decay of luminescence and the exponential fitting graphic representation of the LuAG:0.5%Ce film sample that calcination 2h obtains under 1000 ℃ of temperature.
Embodiment
Specific embodiment of the present invention is specified in the back at present:
Embodiment 1 (preparation LuAG:0.5%Ce film)
With hydrofluoric acid rinsing silicon substrate to remove its surperficial zone of oxidation; Prevent that ionic from staining again; Next successively with acetone, ethanol, water ultrasonic cleaning 20min impurity such as particle with the removal silicon face; Use the vitriol oil and SPA mixing solutions (volume ratio is 3:1) to soak 24h to remove the harmful metal ion of silicon face at last, the monocrystalline silicon piece after the immersion is distinguished water and absolute ethyl alcohol ultrasonic cleaning 10min again to remove the residual acid solution of silicon face.
Take by weighing 1.163g LuCl
36H
2The O powder joins in the 5ml deionized water, adds 1.875g aluminum nitrate and 0.029mlCe (NO by stoichiometric ratio again
3)
3Solution, stirring made powder dissolve fully in 1.5 hours and obtains water white transparency shape solution under 80 ° of C temperature.In gained solution, add an amount of polyoxyethylene glycol (40mg/ml) afterwards, (amount of substance is than being n for Hydrocerol A
Hydrocerol A: n
Metals ion=2:1) and ethanol (volume ratio is V
C2H5OH: V
H2O=8:1), at room temperature stirred 1.5 hours, promptly obtain required precursor colloidal sol.
The monocrystalline silicon piece that cleans up is flat on the microscope carrier of sol evenning machine, the even colloid that leaves standstill is dripped 3-4 with dropper drip to silicon face, regulate the sol evenning machine rotating speed colloid is coated on the substrate equably.The substrate of colloidal sol in the spin coating is transferred to roasting glue machine thermal treatment 5 min under 110 ° of C,, transfers to low temperature oven and heat-treat, remove organism such as surperficial polyoxyethylene glycol and Hydrocerol A to remove surface adsorption water and ethanol.Repetitive operation coating procedure several times obtain the film of desired thickness.Place retort furnace to handle at 800-1100 ° of C temperature lower calcination the precursor film, and be incubated 2 hours, naturally cooling in air finally obtains LuAG:Ce then
3+Film.Fig. 2 is LuAG:Ce
3+Excite and launch spectrogram.
Embodiment 2 (preparation LuAG:1%Ce film)
With hydrofluoric acid rinsing silicon substrate to remove its surperficial zone of oxidation; Prevent that ionic from staining again; Next successively with acetone, ethanol, water ultrasonic cleaning 20min impurity such as particle with the removal silicon face; Use the vitriol oil and SPA mixing solutions (volume ratio is 3:1) to soak 24h to remove the harmful metal ion of silicon face at last, the monocrystalline silicon piece after the immersion is distinguished water and absolute ethyl alcohol ultrasonic cleaning 10min again to remove the residual acid solution of silicon face.
Take by weighing 1.157g LuCl
36H
2The O powder joins in the 5ml deionized water, adds 1.875g aluminum nitrate and 0.057mlCe (NO by stoichiometric ratio again
3)
3Solution, stirring made powder dissolve fully in 1.5 hours and obtains water white transparency shape solution under 80 ° of C temperature.In gained solution, add an amount of polyoxyethylene glycol (40mg/ml) afterwards, (amount of substance is than being n for Hydrocerol A
Hydrocerol A: n
Metals ion=2:1) and ethanol (volume ratio is V
C2H5OH: V
H2O=8:1), at room temperature stirred 1.5 hours, promptly obtain required precursor colloidal sol.
The monocrystalline silicon piece that cleans up is flat on the microscope carrier of sol evenning machine, the even colloid that leaves standstill is dripped 3-4 with dropper drip to silicon face, regulate the sol evenning machine rotating speed colloid is coated on the substrate equably.The substrate of colloidal sol in the spin coating is transferred to roasting glue machine thermal treatment 5 min under 110 ° of C,, transfers to low temperature oven and heat-treat, remove organism such as surperficial polyoxyethylene glycol and Hydrocerol A to remove surface adsorption water and ethanol.Repetitive operation coating procedure several times obtain the film of desired thickness.Place retort furnace to handle at 800-1100 ° of C temperature lower calcination the precursor film, and be incubated 2 hours, naturally cooling in air finally obtains even, transparent, flawless LuAG:Ce then
3+Film.Fig. 3 is the LuAG:Ce of doping different concns cerium ion
3+The emission spectrogram of film.
The various instrument detecting results that done among relevant the present invention list in accompanying drawing.
Fig. 1 is that the XRD figure of the film sample behind the calcining 2h under the differing temps reaches and the PDF card of standard aluminic acid lutetium contrasts.As can be seen from the figure, sample diffraction curve behind 800 ℃ of calcining 2h is a disperse state, shows that precursor does not also begin crystallization under this condition; 900 ℃ of calcinings begin to occur some more weak diffraction peaks behind the 2h, show to begin crystallization the characteristic peak intensity increase of LuAG phase behind 1000 ℃ of calcining 2h; Explain that LuAG forms mutually mostly under this temperature; And along with the rising of temperature, crystallization is more complete, and each diffraction peak is consistent with international standard diffraction card Lu3Al2Al3O12 phase (JCPDS 18-0761); The case that has replaced the part lutetium ion after cerium ion mixes is described, but is not caused the variation of phase.
Fig. 2 is exciting and emmission spectrum figure of calcination 2h obtains under 1000 ℃ of temperature film sample; Can find from PLE; Excitation spectrum is made up of two excitation band peaks, and one is that weak band peak and at center is the strong band peak at center with 442nm with 344nm, and these two band peaks are by Ce
3+Incident radiation absorb and to cause
2F
5/2, 2F
7/2→ 5d
1Jump and caused.Can see that from the emission spectrogram it is that the broad band at center is luminous with 507nm that emmission spectrum is one, this is by Ce
3+Ionic 5d
1The transition emission of-4f broadband is produced.According to the result of Gauss curve fitting, Ce
3+The characteristic emission peak be the broad peak that forms by two peaks (central position is at 495nm and 538nm place) convolution.In addition, we can see, change excitation wavelength, and the position and the shape of its emission peak do not change, and just variation has taken place absorption intensity.Explanation LuAG:Ce film has luminescent properties preferably from this figure.
Fig. 3 is the Lu of the various ce doping content that calcination 2h obtains under 1000 ℃ of temperature
3 (1-X)Al
5O
12: the emmission spectrum figure of xCe (X=0.002,0.005,0.008,0.01) film.From figure, can see that doping content is lower than at 1% o'clock, along with Ce
3+The continuous increase of ion doping concentration, considerable change does not take place in the position of emission peak and shape, is 1% o'clock in doping content, and the position of emission peak and shape have some variation, and its reason is gone back at present and is unclear, but along with Ce
3+Continuous increase and its absorption intensity of ion doping concentration constantly increase.
Fig. 4 is the AFM figure of the film sample that calcination 2h obtains under 1000 ℃ of temperature.(a) plat, (b) three-dimensional plot.From figure, can find that film growth is better, its surfacing, evenly, and flawless, the well-crystallized, its grain size is approximately 80-100nm, and roughness is 1.465nm.
Fig. 5 is the decay of luminescence and the exponential fitting graphic representation of the LuAG:0.5%Ce film sample that calcination 2h obtains under 1000 ℃ of temperature.Can find out that by figure its extinction curve can fit to single index item function:
I?=?I 0 exp(-t/τ)+C (1)
In the formula: I represents relative intensity, I
0Intensity when representing t=0, t represents the fall time corresponding to intensity,
τRepresent damping time constant.
Be 8.8ns its fall time; This powder than LuAG:Ce (20ns) and monocrystalline (63ns) are fast a lot; The LuAG:Ce film is compared with powder and the monocrystalline of LuAG:Ce, and the difference of its fall time mainly is caused by microstructural difference between their threes.Satisfying the requirement of fast decay scintillator so short fall time, is good scintillator material.
Claims (1)
1. Ce
3+Doping aluminic acid lutetium (Lu
3Al
5O
12) preparation method of polycrystalline light emitting film, it is characterized in that this preparation method has following preparation process and step:
(a), the preparation of colloidal sol: according to chemical formula Lu
3 (1-X)Al
5O
12: xCe, x are x, and each element chemistry metering ratio in the chemical formula is pressed in x=0.002～0.01, takes by weighing a certain amount of LuCl
36H
2O (99.99%) powder joins in the 5ml deionized water; Ce (the NO that adds an amount of aluminum nitrate and 0.522mol/L again
3)
3Solution; Under 80 ° of C temperature, stir and made powder dissolve acquisition water white transparency shape solution fully in 1.5 hours; In gained solution, add polyoxyethylene glycol and the Hydrocerol A of an amount of 40mg/ml afterwards, the quality of Hydrocerol A is n with the ratio of the quality of total metals ion
Hydrocerol A: n
Metals ion=2:1; Add aqueous ethanolic solution again, the volume ratio of ethanol and water is V
C2H5OH: V
H2O=8:1; At room temperature stirred 1.5 hours, and promptly obtained required precursor colloidal sol;
(b), the cleaning of silicon substrate: earlier with the zone of oxidation of hydrofluoric acid rinsing 10min with the removal silicon face; Prevent that ionic from staining again; Next successively with acetone, ethanol, water ultrasonic cleaning 20min impurity such as particle with the removal silicon face; Use the vitriol oil and SPA mixing solutions (volume ratio is 3:1) to soak 24h to remove the harmful metal ion of silicon face at last, the monocrystalline silicon piece after the immersion is distinguished water and absolute ethyl alcohol ultrasonic cleaning 10min before use again to remove the residual acid solution of silicon face;
(c), spin coating and thermal pretreatment: the monocrystalline silicon piece that cleans up is flat on the microscope carrier of sol evenning machine, drips 3-4 to the even colloid that leaves standstill with dropper and drip to silicon face, the rotating speed of regulating sol evenning machine makes colloid be coated on the silicon substrate equably; The substrate of colloidal sol in the spin coating is transferred to roasting glue machine thermal treatment 5 min under 110 ° of C,, transfers to low temperature oven and heat-treat, remove organism such as surperficial polyoxyethylene glycol and Hydrocerol A to remove surface adsorption water and ethanol; Repetitive operation coating procedure several times obtain the film of desired thickness;
(d), calcining: will place retort furnace through the precursor thin-film that above-mentioned steps obtains, 800～1100
oThe C temperature lower calcination is handled, and is incubated 1-10 hour, and naturally cooling in air finally obtains even, transparent, flawless Ce then
3+Adulterated LuAG:Ce
3+Film.
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Cited By (3)
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| CN103884664A (en) * | 2014-03-24 | 2014-06-25 | 中国科学院上海硅酸盐研究所 | Method for determining concentration of cerium ions in cerium-doped scintillation crystal |
| CN105293946A (en) * | 2015-11-16 | 2016-02-03 | 宁波大学 | Glass film containing rare-earth-ion-doped Ba2CsBr5 microcrystalline and preparation method thereof |
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2011
- 2011-11-01 CN CN2011103378668A patent/CN102504818A/en active Pending
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| CN105293946A (en) * | 2015-11-16 | 2016-02-03 | 宁波大学 | Glass film containing rare-earth-ion-doped Ba2CsBr5 microcrystalline and preparation method thereof |
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Application publication date: 20120620 |