CN100388405C - Ce-doped Eu-doped lutetium yttrium aluminium acid submicron image screen and its preparation method - Google Patents

Ce-doped Eu-doped lutetium yttrium aluminium acid submicron image screen and its preparation method Download PDF

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CN100388405C
CN100388405C CNB2004100164760A CN200410016476A CN100388405C CN 100388405 C CN100388405 C CN 100388405C CN B2004100164760 A CNB2004100164760 A CN B2004100164760A CN 200410016476 A CN200410016476 A CN 200410016476A CN 100388405 C CN100388405 C CN 100388405C
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heater
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CN1560892A (en
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赵广军
庞辉勇
徐军
夏长泰
何晓明
介明印
周圣明
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Shanghai Institute of Optics and Fine Mechanics of CAS
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Shanghai Institute of Optics and Fine Mechanics of CAS
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Abstract

The present invention relates to a Ce-doped Eu-doped lutetium aluminium acid submicron imaging fluorescent screen and a preparation method thereof. The fluorescent screen is characterized in that the fluorescent screen has the structural formula of Lu(1-x-y)CeyEuxAlO3/LuzY(1-z)AlO3 (0.0001<=x<=0.05, 0.0001<=y<=0.05 and 0<=z<=1). The preparation method of the fluorescent screen comprises: LuzY(1-z)AlO3 with the crystal surface direction of 100 or 001 (0<=z<=1), and a single crystal substrate are used as seed crystals of large areas; a layer of (1-x-y)CeyEuxAlO3 single crystal film of a micron magnitude order and a submicron magnitude order grows on an interface in contact with saturated solution of a fluxing agent with Lu(1-x-y)CeyEuxAlO3 polycrystal materials at the crystallization temperature of Lu(1-x-y)CeyEuxAlO3 single crystal in a liquid phase epitaxial furnace heated by resistance to form the fluorescent screen. The fluorescent screen of the present invention has the characteristics of high quality of the single crystal film, good optical property, high X-ray absorption coefficient and high resolution.

Description

Mix cerium and mix europium lutecium yttrium aluminate sub-micrometer imaging phosphor screen and preparation method thereof
Technical field
The present invention relates to imaging fluorescent screen, particularly a kind of cerium of mixing is mixed europium lutecium yttrium aluminate sub-micrometer imaging phosphor screen and preparation method thereof, and this phosphor screen can be widely used in X-ray detection X fields such as medical science, scientific research, industrial online detection, safety inspection.
Background technology
Sciagraphy is that a kind of employing blinking strengthens screen (scintillation crystal or fluorescent material) and photographic film carries out the method that X ray is surveyed, be a kind of traditional x-ray imaging technology, it has at aspects such as medical diagnosis, metal defect inspections widely uses.But, this traditional sciagraphy have efficient low, waste time and energy, can not carry out shortcoming such as (real-time) observation in real time, be eliminated gradually now.Adopting the photographic film in charge-coupled device (CCD) or amorphous silicon array detectors such as (a-Si:H) the replacement sciagraphy, and show in conjunction with computer control, is one of important trend of X imaging technique development from now on.Compare with traditional sciagraphy, this novel x-ray imaging technology has detection efficient height, digitized degree height, can be implemented in advantage such as line detection in real time, in technical fields such as medical diagnosis on disease, industrial nondestructive testing, astronomical observation, the safety inspection value that has a very wide range of applications.And, development along with the third generation synchrotron radiation light source of the high resonance characteristic of high brightness, this novel x-ray imaging technology also will play an important role in microscopic X-ray imaging fields such as phase contrast imaging, holographic imaging and microtomography, and microscopic X-ray imaging will require system to have micron or the resolution of sub-micron, wider dynamic range and characteristics such as temporal resolution faster.Blinking screen is one of the key factor of the room and time resolution of decision x-ray imaging system.At present, the phosphor screen majority in the imaging system all adopts the phosphor screen of the 2-3 micron thickness that fine fluorescent material (granularity is 1 micron) makes, and this fluoroscopic resolution is general also in the magnitude of 2-3 micron.In addition, because half that the granularity of fluorescent material is big, density only is corresponding crystalline film density, so shortcomings such as the fluorescent phosphor screen exists X ray to absorb and light conversion efficiency is low, fluorescence response time length.In order to improve the resolution of microscopic X-ray imaging, now having developed thickness again only is the phosphor screen of the monocrystalline flicker film (SCF) of micron or submicron order as x-ray imaging system, this SCF phosphor screen will improve the resolution of x-ray imaging greatly, in theory, the resolution of SCF blinking screen can reach the diffraction limit (being about 0.3 micron) of visible light.(referring to: IEEE Trans.Nucl.Sci.1998, the 45th the 3rd phase of volume, the 492nd page; Referring to: J.Opt.Sco.Am.A,, the 15th the 7th phase of volume, the 1940th page in 1998).
Formerly mainly contain SCF phosphor screens such as CsI (T1), Ce:YAG/YAG and Ce:LuAG/YAG in the technology, but these phosphor screens have following shortcoming:
(1) all very little (Z of the effective atomic number of CsI (T1) and Ce:YAG crystal and density EffBe respectively 54.1 and 32, density is respectively 4.52g/cm 3And 4.55g/cm 3), therefore, their X ray absorbability and ray-light conversion efficiency are lower.Must increase the thickness of film in order to improve its resolution, (LSF) knows according to the imaging line spread function, and the increase of thickness will reduce fluoroscopic resolution (resolution is approximately equal to their thickness);
(2) though Ce:LuAG has very big effective atomic number and high density (Z Eff=58.9, density=6.67g/cm 3), but its light output less (3000Ph/Mev);
(3) formerly the emission wavelength of the scintillation single crystal film in the technology in the 480-560nm scope, with the ccd detector coupling efficiency low (peak value of CCD is corresponding to 600-700nm) of present human eye sensitivity;
(4) in addition, the easy deliquescence of CsI (T1) film, its optical attenuation time is grown (900ns), is unsuitable for fast microscopic X-ray imaging in real time.
Summary of the invention
The technical problem to be solved in the present invention is to overcome formerly shortcomings such as SCF phosphor screen low-density in the technology, low light output, long die-away time, low resolution, provide a kind of cerium of mixing to mix europium lutecium yttrium aluminate sub-micrometer imaging phosphor screen and preparation method thereof, phosphor screen of the present invention should have monocrystal thin films quality height, optical property is good, X-ray absorption coefficient is high and resolution is high characteristics.
Technical solution of the present invention is as follows:
A kind of cerium of mixing is mixed europium lutecium yttrium aluminate sub-micrometer imaging phosphor screen, it is characterized in that this fluoroscopic structural formula is Lu 1-x-yCe yEu xAlO 3/ Lu zY 1-zAlO 3, (0.0001≤x≤0.05,0.0001≤y≤0.05,0≤z≤1), this phosphor screen is that crystal plane direction is the Lu of (100) or (010) zY 1 -zAlO 3The substrate monocrystal sheet on one deck Lu of growing 1-x-yCe yEu xAlO 3The compound flash detection material that the scintillation single crystal film constitutes.
Described Lu zY 1-zAlO 3The thickness of substrate monocrystal sheet be the 5-30 micron.
Described Lu 1-x-yCe yEu xAlO 3The thickness of scintillation single crystal film is the 0.3-10 micron.
The described cerium of mixing is mixed the fluoroscopic preparation method of europium lutecium yttrium aluminate sub-micrometer imaging, it is characterized in that this phosphor screen is with the Lu of crystal plane direction for (100) or (001) zY 1-zAlO 3, (0≤z≤1) single crystalline substrate is made the large tracts of land seed crystal, in resistance heating liquid phase epitaxy stove, at Lu 1-x-yCe yEu xAlO 3Under the crystallization temperature of monocrystalline, and contain Lu 1-x-yCe yEu xAlO 3The Lu of growth one deck micron and sub-micrometer scale on the flux saturated solution contact interface of polycrystal material 1-x-yCe yEu xAlO 3Monocrystal thin films and constitute the described Lu that contains 1-x-yCe yEu xAlO 3The raw material proportioning of (0.0001≤x≤0.05,0.0001≤y≤0.05) polycrystal material flux saturated solution is as follows:
1. the set of dispense of flux solution is than being the PbO of 10-13mol and 1mol B 2O 3, or 8-12molBi 2O 3B with 1-3mol 2O 3
2. Lu 1-x-yCe yEu xAlO 3The percentage by weight of (0.0001≤x≤0.05,0.0001≤y≤0.05) polycrystal material and flux is: Lu 1-x-yCe yEu xAlO 3/ flux solution=10wt%-50wt%.
The structure of described resistance heating liquid phase epitaxy stove mainly comprises:
Body of heater (1), body of heater (1) bottom is main furnace body (101), top is annealing body of heater (102), in the main furnace body (101), central authorities are equipped with crucible (9), crucible (9) is coaxial with body of heater (1), relative crucible (9) is provided with side heater (2) on every side in the main furnace body (101), the periphery of side heater (2) is heat insulation layer (11), heat insulation layer (13) is arranged under the crucible (9) and can regulate crucible (9) collet (12) just, upside heater (5) is arranged in the annealing furnace (102), main furnace body (101) also is provided with middle temperature thermocouple (3), and annealing furnace (102) is provided with temperature thermocouple (4), is extended with a rotary pulling bar (6) under the upper top cover mediad of body of heater (1), the lower end of this rotary pulling bar (6) is substrate clamp (7), and rotary pulling bar (6) is coaxial with body of heater (1).
The described cerium of mixing is mixed the fluoroscopic preparation method of europium lutecium yttrium aluminate sub-micrometer imaging, comprises the following steps:
＜1〉according to selected Lu 1-x-yCe yEu xAlO 3The proportioning raw materials weighing of polycrystalline and flux is in the crucible of packing into after fully mixing and in the body of heater of packing into;
＜2〉with crystal plane direction be the Lu of (100) or (010) zY 1-zAlO 3, the substrate wafer of (0≤z≤1) is inserted in the substrate clamp, adjusts the rotary pulling bar and makes it to be on the coaxial position of crucible;
＜3〉programming rate with 100 ℃/Hr is warming up to 1000-1100 ℃, fusion polycrystal raw material Lu 1-x-yCe yEu xAlO 3With flux PbO-B 2O 3Or Bi 2O 3-B 2O 3Make it become saturated solution, treat all dissolvings after, 1100 ℃ of constant temperature 5 hours;
＜4〉the rotary pulling bar that descends gradually drops to from saturated flux liquid level 3-5mm place, again at Lu substrate wafer 1-x-yCe yEu xAlO 3Under the crystallization range 900-1050 ℃ condition constant temperature 2-4 hour;
＜5〉decline rotary pulling bar makes substrate wafer just in time contact saturated solution, and the rotary pulling bar is with the rotation of 100-400r/min speed, according to required growth Lu 1-x-yCe yEu xAlO 3(0.0001≤x≤0.05,0.0001≤y≤0.05) film thickness is regulated corresponding growth time, is generally 3-20 minute, after growth time finishes, mentions the rotary pulling bar immediately and makes substrate break away from liquid level;
＜6〉annealing is mentioned the rotary pulling bar with continuing, and makes substrate wafer and precipitating thereof Lu thereon 1-x-yCe yEu xAlO 3(0.0001≤x≤0.05,0.0001≤y≤0.05) film enters the upside heater interval in the annealing furnace, the power of heater in the adjustment makes its temperature after 900 ℃ of constant temperature 30-60 minutes, be cooled to room temperature with 50 ℃/Hr speed then, finish the fluoroscopic preparation of scintillation single crystal.
Described step＜5〉before the decline rotary pulling bar, should adjust the heating power of the side heater of main furnace body, temperature thermocouple is designated as 900-1050 ℃, the rotary pulling of constant temperature 1-2h, and then decline again bar in making.
Technique effect of the present invention is as follows:
1, shows Lu of the present invention after tested 1-x-yCe yEu xAlO 3/ Lu zY 1-zAlO 3, (0.0001≤x≤0.05,0.0001≤y≤0.05,0≤z≤1) fluoroscopic emission wavelength can more effectively be coupled with existing C CD near 600-700nm.The fluoroscopic effective atomic number Z of the present invention Eff≈ 65, density p ≈ 8.3g/cm 3, fluoroscopic light output is about 30-40%NaI (T1).
2, Lu of the present invention 1-x-yCe yEu xAlO 3/ Lu zY 1-zAlO 3(0.0001≤x≤0.05,0.0001≤y≤0.05,0≤z≤1) phosphor screen can be coupled with CCD and Si array (a-Si:H), can survey rays such as X ray, gamma rays, the X ray micro imaging system of the submicron order that constitutes can be widely used in fields such as medical treatment, industry, safety check and scientific research.
3, the present invention compared with prior art, on the one hand because cerium, europium ion-doped aluminic acid lutetium monocrystalline Lu 1-x-yCe yEu xAlO 3(0.0001≤x≤0.05,0.0001≤y≤0.05) has heavy density (8.3g/cm 3), high effective atomic number (66), high light output (12000Ph/Mve), fast decay advantages such as (18-30ns), therefore, phosphor screen of the present invention more formerly in the technology phosphor screen have higher X-ray absorption coefficient, higher resolution; On the other hand, the isoelectronic ion Ce that radius is bigger 3+, Eu 3+Adding, can be so that the mismatch degree between film and the substrate reduces greatly, the monocrystal thin films quality improves, fluoroscopic optical property might as well.In addition, this fluoroscopic emission wavelength has better coupling with CCD about 600-700nm, can improve its response efficiency.
Therefore, adopt blinking screen of the present invention can be widely used in various microscopic X-ray imaging fields.
Description of drawings
Fig. 1 is that the present invention prepares Lu 1-x-yCe yEu xAlO 3/ Lu zY 1-zAlO 3, the resistance heating liquid phase epitaxy stove generalized section of (0.0001≤x≤0.05,0.0001≤y≤0.05,0≤z≤1) blinking screen growth.
Fig. 2 is the LuAlO that the present invention Ce, the Eu that prepare mix 3The spectrogram of the 600-700nm scope that monocrystal thin films is launched under the 246nm shooting condition.
Embodiment
See also Fig. 1 earlier, Fig. 1 is that the present invention prepares Lu 1-x-yCe yEu xAlO 3/ Lu zY 1-zAlO 3, the resistance heating liquid phase epitaxy stove generalized section of (0.0001≤x≤0.05,0.0001≤y≤0.05,0≤z≤1) blinking screen growth.As seen from the figure, the present invention prepares Lu 1-x-yCe yEu xAlO 3/ Lu zY 1-zAlO 3, the structure of the employed resistance heating liquid phase epitaxy of (0.0001≤x≤0.05,0.0001≤y≤0.05,0≤z≤1) blinking screen method stove mainly comprises:
Body of heater 1, body of heater 1 bottom is a main furnace body 101, upper of furnace body is an annealing body of heater 102.Central authorities are equipped with crucible 9 in body of heater 1, crucible 9 and body of heater 1 concentricity axis.Crucible 9 is built-in with and contains Lu 1-x-yCe yEu xAlO 3(0.0001≤x≤0.05,0.0001≤y≤0.05) polycrystal material and PbO-B 2O 3Or Bi 2O 3-B 2O 3Cosolvent saturated solution 10.Under stretch on body of heater top, rotary pulling bar 6 is arranged, substrate clamp 7 is arranged, on substrate clamp 7, be equipped with Lu in the lower end of rotary pulling bar 6 zY 1 -zAlO 3, (0≤z≤1) substrate wafer puts in 9 li in crucible.Rotary pulling bar 6 and body of heater 1 concentricity axis.Around the crucible 9 of main furnace body 101, side heater 5 is arranged,, heat insulation layer 13 is arranged under crucible 9 and the collet 12 that can regulate the crucible height is arranged at the outer heat insulation layer 13 that is with of side heater 5.In the annealing furnace 102 of upper of furnace body, upside heater 5 is arranged.Thermometric thermocouple 3 in also having in the device, last thermometric thermocouple 4 etc.In body of heater, after annealing furnace 5 annealing, can eliminate fluoroscopic thermal stress, prevent cracking.
The Lu that preparation method of the present invention adopted 1-x-yCe yEu xAlO 3(0.0001≤x≤0.05,0.0001≤y≤0.05) polycrystal material flux saturated solution is by Lu 1-x-yCe yEu xAlO 3Polycrystal material and flux lead oxide (PbO) and diboron trioxide (B 2O 3) or bismuth oxide (Bi 2O3) and diboron trioxide (B 2O 3) by following proportioning system:
Flux PbO and B 2O 3Mol ratio be PbO: B 2O 3=(10-13) mol: 1mol; Or take flux Bi 2O 3With B 2O 3, its ratio is Bi 2O 3: B 2O 3=(8-12) mol: (1-3mol);
Lu 1-x-yCe yEu xAlO 3The percentage by weight of (0.0001≤x≤0.05,0.0001≤y≤0.05) polycrystalline and flux is: Lu 1-x-yCe yEu xAlO 3/ flux=10wt%-50wt%
Now the invention will be further described in conjunction with following specific embodiment.
Embodiment 1:Lu 0.9998Ce 0.0001Eu 0.0001AlO 3/ YAlO 3Phosphor screen
Selected resistance heating liquid phase epitaxy stove device as shown in Figure 1, the crucible 9 in the main body stove 101 is a platinum crucible.According to above-mentioned step of preparation process＜1〉with polycrystal raw material Lu 0.9998Ce 0.0001Eu 0.0001AlO 3With cosolvent (PbO: B2O3=10mol: 1mol) be Lu by weight percentage 0.9998Ce 0.0001Eu 0.0001AlO 3/ (PbO+B2O3)=0.20 proportioning is carried out weighing 1000g altogether, packs into after mixing
Figure C20041001647600111
In the platinum crucible 9 of 80 * 80mm;
By processing step＜2〉will be of a size of
Figure C20041001647600112
30 * 0.03mm, crystal plane direction is the YAlO of (100) 3Substrate 8 places in the anchor clamps 7, and with anchor clamps 7 rotary pulling bar 6 bottoms of packing into, and the position of adjusting crucible 9 and substrate wafer 8 makes it coaxial, and all is in the central authorities of main furnace body 101;
By above-mentioned steps＜3〉body of heater 101 is warming up to 1100 ℃, make raw material and flux be melt into saturated solution 10, and 1100 ℃ of constant temperature 5 hours;
The rotary pulling bar 6 that descends gradually set by step＜4〉makes substrate wafer 8 apart from saturated liquid level 4mm, again at Lu 0.9998Ce 0.0001Eu 0.0001AlO 3Constant temperature is 3 hours under 1050 ℃ of temperature of crystallization range;
By above-mentioned processing step＜5〉decline rotary pulling bar 6 just contacts in the saturated solution 10 substrate wafer 8, and rotary pulling bar 6 is rotated with 300r/min speed, after constant temperature under 1050 ℃ of temperature was grown 5 minutes, lift from rapidly rotary pulling bar 6 make substrate wafer and on monocrystalline break away from liquid level, crystallization is so far finished;
By above-mentioned processing step＜6〉anneal, with the Lu of growth 0.9998Ce 0.0001Eu 0.0001AlO 3Monocrystalline lifts to heater 5 intervals of body of heater 1 top annealing furnace 102 together with substrate wafer 8, and constant temperature was cooled to room temperature with 50 ℃/Hr speed after 30 minutes under 900 ℃ of temperature, and annealing finishes, Lu 0.9998Ce 0.0001Eu 0.0001AlO 3/ YAlO 3The preparation of blinking screen finishes.
Embodiment 2:Lu 0.998Ce 0.01Eu 0.01AlO 3/ LuAlO 3The blinking screen
According to step＜1 in the foregoing description 1〉with Lu 0.998Ce 0.01Eu 0.01AlO 3Polycrystal material and cosolvent (Bi203: B203=8mol: 2mol) be Lu by weight percentage 0.998Ce 0.01Eu 0.01AlO 3/ (Bi203+B203)=0.40 proportioning is carried out weighing 1000g altogether, presses step in the foregoing description 1＜2 〉, will be of a size of φ 20 * 0.03mm, crystal plane direction is the LuAlO of (001) 3Substrate 8 places in the anchor clamps 7, and with anchor clamps 7 rotary pulling bar 6 bottoms of packing into, and the position of adjusting crucible 9 and substrate wafer 8 makes it coaxial, and all is in the central authorities of main furnace body 101; By in the foregoing description 1＜3 body of heater 101 is warming up to 1100 ℃, make raw material and flux be melt into saturated solution 10, and at 1100 ℃ of constant temperature after 5 hours, by in the foregoing description 1＜4 rotary pulling bar 6 gradually descends, make substrate wafer 8 apart from saturated liquid level 3mm, again at Lu 0.998Ce 0.01Eu 0.01AlO 3Constant temperature is 3 hours under 1030 ℃ of temperature of crystallization range, by in the foregoing description 1＜5〉decline rotary pulling bars 6 make an end face of substrate wafer 8 contact with saturated solution 10 liquid levels, and rotary pulling bar 6 is rotated with 200r/min speed, after constant temperature under 1030 ℃ of temperature was grown 10 minutes, lift from rapidly rotary pulling bar 6 make substrate wafer and on monocrystalline break away from liquid level, crystallization is so far finished; Step＜6 by the foregoing description 1〉anneal, be about to the Lu of growth 0.998Ce 0.01Eu 0.01AlO 3Monocrystalline lifts to the hot zone of body of heater 1 top annealing furnace 102 together with substrate wafer 8, and constant temperature was cooled to room temperature with 50 ℃/Hr speed after 1 hour under 900 ℃ of temperature, and annealing finishes; Finish Lu 0.998Ce 0.01Eu 0.01AlO 3/ LuAlO 3The preparation of blinking screen.
Embodiment 3:Lu 0.99Eu 0.05Ce 0.05AlO 3/ Lu 0.8Y 0.2AlO 3The blinking screen
According to step＜1 in the foregoing description 2〉with Lu 0.99Eu 0.05Ce 0.05AlO 3Polycrystal material and cosolvent (Bi203: B203=8mol: 2mol) be Lu by weight percentage 0.99Eu 0.05Ce 0.05AlO 3/ (Bi203+B203)=0.50 proportioning is carried out weighing 1000g altogether, presses step in the foregoing description 2＜2 〉, will be of a size of φ 20 * 0.03mm, crystal plane direction is the Lu of (100) 0.8Y 0.2AlO 3Substrate 8 places in the anchor clamps 7, and with anchor clamps 7 rotary pulling bar 6 bottoms of packing into, and the position of adjusting crucible 9 and substrate wafer 8 makes it coaxial, and all is in the central authorities of main furnace body 101; By in the foregoing description 2＜3 body of heater 101 is warming up to 1150 ℃, make raw material and flux be melt into saturated solution 10, and at 1150 ℃ of constant temperature after 5 hours, by in the foregoing description 2＜4 rotary pulling bar 6 gradually descends, make substrate wafer 8 apart from saturated liquid level 3mm, again at Lu 0.99Eu 0.05Ce 0.05AlO 3Constant temperature is 3 hours under 1040 ℃ of temperature of crystallization range, by in the foregoing description 2＜5〉decline rotary pulling bars 6 make the end face of substrate wafer 8 contact with saturated solution 10 liquid levels, and rotary pulling bar 6 is rotated with 400r/min speed, after constant temperature under 1040 ℃ of temperature was grown 5 minutes, lift from rapidly rotary pulling bar 6 make substrate wafer and on monocrystalline break away from liquid level, crystallization is so far finished; Step＜6 by the foregoing description 2〉anneal, be about to the Lu of growth 0.697Y 0.3Ce 0.003AlO 3Monocrystalline lifts to the hot zone of body of heater 1 top annealing furnace 102 together with substrate wafer 8, and constant temperature was cooled to room temperature with 50 ℃/Hr speed after 50 minutes under 900 ℃ of temperature, and annealing finishes; Finish Lu 0.99Eu 0.05Ce 0.05AlO 3/ Lu 0.8Y 0.2AlO 3The preparation of blinking screen blinking screen.
This blinking screen has higher resolution, and it can be widely used in applications such as medical science, holographic imaging, phase contrast imaging.

Claims (7)

1. mix cerium and mix europium lutecium yttrium aluminate sub-micrometer imaging phosphor screen for one kind, it is characterized in that this fluoroscopic structural formula is Lu 1-x-yCe yEu xAlO 3/ Lu zY 1-zAlO 3, (0.0001≤x≤0.05,0.0001≤y≤0.05,0≤z≤1), this phosphor screen is that crystal plane direction is the Lu of (100) or (010) zY 1-zAlO 3The substrate monocrystal sheet on one deck Lu of growing 1-x-yCe yEu xAlO 3The compound flash detection material that the scintillation single crystal film constitutes.
2. the cerium of mixing according to claim 1 is mixed europium lutecium yttrium aluminate sub-micrometer imaging phosphor screen, it is characterized in that described Lu zY 1-zAlO 3The thickness of substrate monocrystal sheet be the 5-30 micron.
3. the cerium of mixing according to claim 1 is mixed europium lutecium yttrium aluminate sub-micrometer imaging phosphor screen, it is characterized in that described Lu 1-x-yCe yEu xAlO 3The thickness of scintillation single crystal film is the 0.3-10 micron.
4. one kind prepares the described cerium of mixing of claim 1 and mixes the fluoroscopic method of europium lutecium yttrium aluminate sub-micrometer imaging, it is characterized in that this phosphor screen is with the Lu of crystal plane direction for (100) or (001) zY 1-zAlO 3, (0≤z≤1) single crystalline substrate is made the large tracts of land seed crystal, in resistance heating liquid phase epitaxy stove, at Lu 1-x-yCe yEu xAlO 3Under the crystallization temperature of monocrystalline, and contain Lu 1-x-yCe yEu xAlO 3The Lu of growth one deck micron and sub-micrometer scale on the flux saturated solution contact interface of polycrystal material 1-x-yCe yEu xAlO 3Monocrystal thin films and constitute the described Lu that contains 1-x-yCe yEu xAlO 3The raw material proportioning of (0.0001≤x≤0.05,0.0001≤y≤0.05) polycrystal material flux saturated solution is as follows:
1. the set of dispense of flux solution is than the B for the PbO of 10-13mol and 1mol 2O 3, or the Bi of 8-12mol 2O 3B with 1-3mol 2O 3
2. Lu 1-x-yCe yEu xAlO 3The percentage by weight of (0.0001≤x≤0.05,0.0001≤y≤0.05) polycrystal material and flux is: Lu 1-x-yCe yEu xAlO 3/ flux solution=10wt%-50wt%.
5. the cerium of mixing according to claim 4 is mixed the fluoroscopic preparation method of europium lutecium yttrium aluminate sub-micrometer imaging, it is characterized in that the structure of described resistance heating liquid phase epitaxy stove mainly comprises:
Body of heater (1), body of heater (1) bottom is main furnace body (101), top is annealing body of heater (102), in the main furnace body (101), central authorities are equipped with crucible (9), crucible (9) is coaxial with body of heater (1), relative crucible (9) is provided with side heater (2) on every side in the main furnace body (101), the periphery of side heater (2) is heat insulation layer (11), heat insulation layer (13) is arranged under the crucible (9) and can regulate crucible (9) collet (12) just, upside heater (5) is arranged in the annealing furnace (102), main furnace body (101) also is provided with middle temperature thermocouple (3), and annealing furnace (102) is provided with temperature thermocouple (4), is extended with a rotary pulling bar (6) under the upper top cover mediad of body of heater (1), the lower end of this rotary pulling bar (6) is substrate clamp (7), and rotary pulling bar (6) is coaxial with body of heater (1).
6. the cerium of mixing according to claim 5 is mixed the fluoroscopic preparation method of europium lutecium yttrium aluminate sub-micrometer imaging, it is characterized in that described this method comprises the following steps:
＜1〉according to selected Lu 1-x-yCe yEu xAlO 3The proportioning raw materials weighing of polycrystalline and flux is in the crucible (9) of packing into after fully mixing and in the body of heater of packing into (1);
＜2〉with crystal plane direction be the Lu of (100) or (010) zY 1-zAlO 3, the substrate wafer (8) of (0≤z≤1) is inserted in the substrate clamp (7), adjusts rotary pulling bar (6) and makes it to be on the coaxial position of crucible (9);
＜3〉programming rate with 100 ℃/Hr is warming up to 1000-1100 ℃, fusion polycrystal raw material Lu 1-x-yCe yEu xAlO 3With flux PbO-B 2O 3Or Bi 2O 3-B 2O 3Make it become saturated solution (10), treat all dissolvings after, 1100 ℃ of constant temperature 5 hours;
＜4〉the rotary pulling bar (6) that descends gradually drops to from saturated flux liquid level 3-5mm place, again at Lu substrate wafer (8) 1-x-yCe yEu xAlO 3Under the crystallization range 900-1050 ℃ condition constant temperature 2-4 hour;
＜5〉decline rotary pulling bar (6) makes substrate wafer (8) just in time contact saturated solution (10), and rotary pulling bar (6) is with the rotation of 100-400r/min speed, according to required growth Lu 1-x-yCe yEu xAlO 3(0.0001≤x≤0.05,0.0001≤y≤0.05) film thickness is regulated corresponding growth time, is generally 3-20 minute, and growth time is mentioned rotary pulling bar (6) after finishing immediately, makes substrate (8) break away from liquid level;
＜6〉annealing is mentioned rotary pulling bar (6) with continuing, and makes substrate wafer (8) and precipitating Lu thereon thereof 1-x-yCe yEu xAlO 3(0.0001≤x≤0.05,0.0001≤y≤0.05) film enters upside heater (5) interval in the annealing furnace (102), adjusts the power of upside heater (5), makes its temperature after 900 ℃ of constant temperature 30-60 minutes, be cooled to room temperature with 50 ℃/Hr speed then, finish Lu 1-x-yCe yEu xAlO 3/ Lu zY 1-zAlO 3, the fluoroscopic preparation of (0.0001≤x≤0.05,0.0001≤y≤0.05,0≤z≤1) scintillation single crystal.
7. the cerium of mixing according to claim 6 is mixed the fluoroscopic preparation method of europium lutecium yttrium aluminate sub-micrometer imaging, it is characterized in that described step＜5〉decline rotary pulling bar (6) is before, should adjust the heating power of the side heater (2) of main furnace body (101), make middle temperature thermocouple (3) be designated as 900-1050 ℃, the rotary pulling of constant temperature 1-2h, and then decline again bar (6).
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CN1146478A (en) * 1995-06-28 1997-04-02 罗纳·布朗克化学公司 Compound based rare-earth phosphate used as luminous material in plasma system
CN1328526A (en) * 1998-09-03 2001-12-26 罗狄亚化学公司 Lanthanum, lutetium, yttrium or gadolinium borate comprising two doping agents and its precursor use in plasma or x-ray systems
CN1390987A (en) * 2002-07-26 2003-01-15 中国科学院上海光学精密机械研究所 Composite flash crystal doped by lutetium cerialuminate and yttrium aluminate and its preparing process
CN1390988A (en) * 2002-07-26 2003-01-15 中国科学院上海光学精密机械研究所 Process for preparing polycrystal doped by three-valence Ce ions, yttrium aluminate, lutetium aluminate and lutetium yttrium aluminate

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1116667A (en) * 1964-05-28 1968-06-12 Sylvania Electric Prod Cathodo-luminescent screens and phosphors therefor
CN1097454A (en) * 1992-01-13 1995-01-18 麦克凯尔桑有限公司 Luminescent material
CN1146478A (en) * 1995-06-28 1997-04-02 罗纳·布朗克化学公司 Compound based rare-earth phosphate used as luminous material in plasma system
CN1328526A (en) * 1998-09-03 2001-12-26 罗狄亚化学公司 Lanthanum, lutetium, yttrium or gadolinium borate comprising two doping agents and its precursor use in plasma or x-ray systems
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