CN1560890A - Cerium doped lutetium yttrium aluminium acid submicron imaging screen and its preparation method - Google Patents
Cerium doped lutetium yttrium aluminium acid submicron imaging screen and its preparation method Download PDFInfo
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- CN1560890A CN1560890A CNA2004100164741A CN200410016474A CN1560890A CN 1560890 A CN1560890 A CN 1560890A CN A2004100164741 A CNA2004100164741 A CN A2004100164741A CN 200410016474 A CN200410016474 A CN 200410016474A CN 1560890 A CN1560890 A CN 1560890A
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- 238000003384 imaging method Methods 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- ANDNPYOOQLLLIU-UHFFFAOYSA-N [Y].[Lu] Chemical compound [Y].[Lu] ANDNPYOOQLLLIU-UHFFFAOYSA-N 0.000 title claims description 14
- 229910052684 Cerium Inorganic materials 0.000 title description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title description 2
- 239000002253 acid Substances 0.000 title 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title 1
- 229910052782 aluminium Inorganic materials 0.000 title 1
- 239000004411 aluminium Substances 0.000 title 1
- 239000000758 substrate Substances 0.000 claims abstract description 47
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 239000010408 film Substances 0.000 claims abstract description 17
- 239000012047 saturated solution Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 11
- 230000008025 crystallization Effects 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 6
- 239000010409 thin film Substances 0.000 claims abstract description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 26
- 230000004907 flux Effects 0.000 claims description 25
- 238000000137 annealing Methods 0.000 claims description 21
- 230000004397 blinking Effects 0.000 claims description 14
- VXLGWCOZCKOULK-UHFFFAOYSA-K aluminum;cerium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Al].[Ce+3] VXLGWCOZCKOULK-UHFFFAOYSA-K 0.000 claims description 13
- 230000012010 growth Effects 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 10
- 230000007423 decrease Effects 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 238000004943 liquid phase epitaxy Methods 0.000 claims description 9
- 238000009413 insulation Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000012856 packing Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 230000004927 fusion Effects 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000007791 liquid phase Substances 0.000 abstract 1
- -1 lutetium yttrium lutetium aluminate Chemical class 0.000 abstract 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 13
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 8
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 6
- 239000006184 cosolvent Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000007689 inspection Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000011555 saturated liquid Substances 0.000 description 3
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 3
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000003745 diagnosis Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000010603 microCT Methods 0.000 description 1
- 238000009659 non-destructive testing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000005469 synchrotron radiation Effects 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Luminescent Compositions (AREA)
- Measurement Of Radiation (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A Ce-doped lutetium yttrium lutetium aluminate submicron imaging screen and its preparation method, the structure of the screen is Lu with (010), (100) or (001) crystal face direction1－zYzAlO3Growing a layer of scintillation film Lu on the substrate1－x－yCeyYxAlO3Wherein x is more than or equal to 0 and less than or equal to 0.9999, y is more than or equal to 0.0001 and less than or equal to 0.05, and z is more than or equal to 0 and less than or equal to 1), and the preparation method of the fluorescent screen comprises the step of preparing Lu with the crystal face direction of (010), (100) or (001)1－zYzAlO3(z is more than or equal to 0 and less than or equal to 1) using the single crystal substrate as a large-area seed crystal in a resistance heating liquid phase epitaxial furnace in LuzY1－zAlO3At the crystallization temperature of the single crystal with a solution containing Lu1－x－yCeyYxAlO3Growing a layer of micron and submicron Lu on the contact interface of the polycrystalline material and the saturated solution of the fluxing agent1－x－yCeyYxAlO3A single crystal thin film. The fluorescent screen has high efficiency and high resolution.
Description
Technical field
The present invention relates to a kind of X ray sub-micrometer imaging phosphor screen, particularly a kind of Cerium aluminate lutetium yttrium sub-micrometer imaging phosphor screen and preparation method thereof of mixing, this phosphor screen can be widely used in the 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, and value has a very wide range of applications in technical fields such as medical diagnosis on disease, industrial nondestructive testing, astronomical observation, safety inspection.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 5th 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 (Tl), Ce:YAG/YAG and Ce:LuAG/YAG in the technology, but these phosphor screens has following shortcoming: all very little (Z of the effective atomic number of (1) CsI (Tl) 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), and, LuAG and bigger as lattice mismatch degree between the YAG of substrate, this is unfavorable for the monocrystal thin films of growing high-quality on substrate, this will have a strong impact on fluoroscopic optical property; (3) in addition, the easy deliquescence of CsI (Tl) film, its optical attenuation time is grown (600ns), is unsuitable for fast microscopic X-ray imaging in real time; (4) in addition, formerly the resolution of the SCF film in the technology is all less relatively, is about the 0.7-0.8 micron.
Summary of the invention
The technical problem to be solved in the present invention is the shortcoming that overcomes SCF phosphor screen low-density in the technology formerly, low light output, long die-away time, low resolution etc., and a kind of Cerium aluminate lutetium yttrium sub-micrometer imaging phosphor screen and preparation method thereof of mixing is provided.This phosphor screen should have high efficiency and high-resolution characteristics.
Technical solution of the present invention is as follows:
A kind of Cerium aluminate lutetium yttrium sub-micrometer imaging phosphor screen of mixing, this fluoroscopic structure are at the Lu of crystal plane direction for (010), (100) or (001)
1-zY
zAlO
3Growth one deck flicker film Lu on (0≤z≤1) substrate
1-x-yCe
yY
xAlO
3And constitute i.e. Lu
1-x-yCe
yY
xAlO
3/ Lu
1-zY
zAlO
3(0≤x≤0.9999,0.0001≤y≤0.05,0≤z≤1).
Described Lu
1-zY
zAlO
3The thickness of (0≤z≤1) substrate is the 5-30 micron, described flicker film Lu
1-x-yCe
yY
zAlO
3Thickness be the 0.3-10 micron.
The described fluoroscopic preparation method of Cerium aluminate lutetium yttrium sub-micrometer imaging that mixes is characterized in that this phosphor screen is with the Lu of crystal plane direction for (010), (100) or (001)
1-zY
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
zY
1-zAlO
3Under the crystallization temperature of monocrystalline, and contain Lu
1-x-yCe
yY
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
yY
xAlO
3Monocrystal thin films.
The described Lu that contains
1-x-yCe
yY
xAlO
3The raw material proportioning of (0≤x≤0.9999,0.0001≤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 8-15mol and 1mol B
2O
3, or 10-12molBi
2O
3B with 1-3mol
2O
3
2. Lu
1-x-yCe
yY
xAlO
3The percentage by weight of (0≤x≤0.9999,0.0001≤y≤0.05) polycrystalline and flux is: Lu
1-x-yCe
yY
xAlO
3/ flux solution=10wt%-50wt%
The structure of described resistance heating liquid phase epitaxy stove mainly comprises:
Body of heater, the body of heater bottom is a main furnace body, upper of furnace body is the annealing body of heater, in body of heater, central authorities are equipped with crucible, crucible is coaxial with body of heater, be provided with the side heater around the crucible relatively in the main furnace body, the periphery of side heater is a heat insulation layer, heat insulation layer is arranged under the crucible and can regulate crucible collet just, the upside heater is arranged in the annealing furnace, main furnace body also is provided with middle temperature thermocouple, and annealing furnace is provided with temperature thermocouple, extends a rotary pulling bar under the upper top cover mediad of body of heater, the lower end of this rotary pulling bar is a substrate clamp, and the rotary pulling bar is coaxial with body of heater.
The described fluoroscopic preparation method of Cerium aluminate lutetium yttrium sub-micrometer imaging that mixes comprises the following steps:
＜1〉according to selected Lu
1-x-yCe
yY
xAlO
3The proportioning raw materials weighing of polycrystalline and flux is in the crucible of the resistance heating liquid phase epitaxy stove 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) or (001)
1-zY
zAlO
3The substrate wafer of (0≤z≤1) is inserted in the substrate clamp, adjusts the rotary pulling bar, makes it to be on the coaxial position of crucible;
＜3〉programming rate with 100 ℃/Hr is warming up to 1050-1200 ℃, fusion polycrystal raw material Lu
1-x-yCe
yY
xAlO
3With flux PbO-B2O3 or Bi2O3-B2O3; Make it become saturated solution (10), treat all dissolvings after, 1100-1250 ℃ 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
yY
xAlO
3Under the crystallization range 900-1150 ℃ condition constant temperature 2-4 hour;
＜5〉decline rotary pulling bar just in time contacts in the saturated solution substrate wafer, and the rotary pulling bar is with the rotation of 100-400r/min speed, according to required growth Lu
1-x-yCe
yY
xAlO
3(0≤x≤0.9999,0.0001≤y≤0.05) film thickness is regulated corresponding growth time, is generally 3-20 minute, and growth time is mentioned the rotary pulling bar after finishing immediately, 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
yY
xAlO
3(0≤x≤0.9999,0.0001≤y≤0.05) film enters the upside heater interval in the annealing furnace, and the power of heater makes its temperature after 900 ℃ of constant temperature 30-60 minutes in the adjustment, is cooled to room temperature with 50 ℃/hr speed then, finishes Lu
1-x-yCe
yY
xAlO
3/ Lu
1-zY
zAlO
3The preparation of (0≤x≤0.9999,0.0001≤y≤0.05,0≤z≤1) blinking screen.
Described step＜5〉before the decline rotary pulling bar, adjust the heating power of the side heater of main furnace body earlier, temperature thermocouple is designated as 900-1150 ℃, the rotary pulling of constant temperature 1-2h, and then decline again bar (6) in making.
Technique effect of the present invention is as follows:
The present invention compared with prior art, on the one hand because cerium ion-doped lutecium yttrium aluminate monocrystalline Lu
1-x-yCe
yY
xAlO
3(0≤x≤0.9999,0.0001≤y≤0.05) has heavy density (along with the density that reduces of x is increased to 8.6g/cm from 5.4
3), the output of high effective atomic number, high light is (along with x increases and increases, 12000Ph/Mve and 15000Ph/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, substrate adopts with the scintillation single crystal film forms identical monocrystalline composition, does not have mismatch, monocrystal thin films quality height, and fluoroscopic optical property is good.In addition, this fluoroscopic emission wavelength is about 370nm, and its diffraction limit is littler, so more helps improving fluoroscopic resolution (being generally sub-micron).
Therefore, adopt blinking screen of the present invention can be widely used in the various microscopic X-ray imaging fields.
Description of drawings
Fig. 1 is that the present invention prepares Lu
1-x-yCe
yY
xAlO
3/ Lu
1-zY
zAlO
3The resistance heating liquid phase epitaxy stove generalized section that (0≤x≤0.9999,0.0001≤y≤0.05,0≤z≤1) blinking screen is used.
Embodiment
See also Fig. 1 earlier, as seen from the figure, the present invention prepares Lu
1-x-yCe
yY
xAlO
3/ Lu
1-zY
zAlO
3The structure of the employed resistance heating liquid phase epitaxy of (0≤x≤0.9999,0.0001≤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, body of heater 1 top is annealing body of heater 102.In body of heater 101, central authorities are equipped with crucible 9, crucible 9 is coaxial with body of heater 1, be provided with side heater 2 around the crucible 9 relatively in the main furnace body 101, the periphery of side heater 2 is a 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, annealing furnace 102 is provided with temperature thermocouple, be 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 a substrate clamp 7, and rotary pulling bar 6 is coaxial with body of heater 1.
Put in the crucible 9 and contain Lu
1-x-yCe
yY
xAlO
3(0≤x≤0.9999,0.0001≤y≤0.05) polycrystal material and PbO-B
2O
3Or Bi
2O
3-B
2O
3The cosolvent saturated solution.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 of main furnace body 101, side heater 2 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 11 that is with of side heater.In the annealing furnace 102 on body of heater 1 top, upside heater 5 is arranged.Thermometric thermocouple 3 in also having in the device, last thermometric thermocouple 4 etc.Thermal stress in the phosphor screen that annealing furnace 102 feasible growths in apparatus of the present invention in the body of heater 1 finish is to prevent cracking etc.
The Lu that preparation method of the present invention adopted
1-x-yCe
yY
xAlO
3(0≤x≤0.9999,0.0001≤y≤0.05) polycrystal material flux saturated solution is by Lu
1-x-yCe
yY
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: B2O3=(8-15) mol: 1mol; Or take flux Bi
2O
3With B
2O
3, its ratio is Bi
2O
3: B
2O
3=(10-12) mol: (1-3mol);
Lu
1-x-yCe
yY
xAlO
3The percentage by weight of (0≤x≤0.9999,0.0001≤y≤0.05) polycrystalline and flux is: Lu
1-x-yCe
yY
xAlO
3/ flux=10wt%-50wt%
Now the invention will be further described in conjunction with following specific embodiment.
Embodiment 1:Lu
0.9999Ce
0.0001AlO
3/ luAlO
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
0.9999Ce
0.0001AlO
3With cosolvent (PbO: B2O3=10mol: 1mol) be Lu by weight percentage
0.9999Ce
0.0001AlO
3/ (PbO+B2O3)=0.20 proportioning is carried out weighing 1000g altogether, in the platinum crucible 9 of the φ 80 * 80mm that packs into after mixing; By processing step＜2〉will be of a size of φ 30 * 0.03mm, crystal plane direction is the LuAlO of (010)
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 1150 ℃, make raw material and flux be melt into saturated solution 10, and at 1150 ℃ of constant temperature after 5 hours, set by step＜4 the rotary pulling bar 6 that descends gradually, make substrate wafer 8 apart from saturated liquid level 4mm, again at Lu
0.9999Ce
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
0.9999Ce
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
0.9999Ce
0.0001AlO
3/ luAlO
3The preparation of blinking screen finishes.
This blinking screen is with a wide range of applications aspect microscopic X-ray imaging.
Embodiment 2:Y
0.9999Ce
0.0001AlO
3/ YAlO
3Phosphor screen
According to step＜1 in the foregoing description 1〉with Y
0.9999Ce
0.0001AlO
3Polycrystal material and cosolvent (Bi2O3: B2O3=8mol: 2mol) be Y by weight percentage
0.9999Ce
0.0001AlO
3/ (Bi2O3+B2O3)=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 YAlO 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 Y
0.9999Ce
0.0001AlO
3Constant temperature is 3 hours under 1000 ℃ 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 1000 ℃ 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 Y of growth
0.9999Ce
0.0001AlO
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 Y
0.9999Ce
0.0001AlO
3/ YAlO
3The preparation of blinking screen.
Embodiment 3:Y
0.995Ce
0.005AlO
3/ YAlO
3Phosphor screen
According to step＜1 in the foregoing description 2〉with Y
0.9999Ce
0.005AlO
3Polycrystal material and cosolvent (Bi2O3: B2O3=10mol: 1mol) be Y by weight percentage
0.995Ce
0.005AlO
3/ (Bi2O3+B2O3)=0.40 proportioning is carried out weighing 1000g altogether, repeats step＜2 in the foregoing description 2 〉,＜3 〉,＜4〉and,＜5 〉,＜6 〉.Finish Y at last
0.995Ce
0.005AlO
3/ YAlO
3The preparation of blinking screen.
Embodiment 4:Lu
0.697Y
0.3Ce
0.003AlO
3/ Lu
0.7Y
0.3AlO
3Phosphor screen
According to step＜1 in the foregoing description 2〉with Lu
0.697Y
0.3Ce
0.003AlO
3Polycrystal material and cosolvent (Bi2O3: B2O3=8mol: 2mol) be Lu by weight percentage
0.697Y
0.3Ce
0.003AlO
3/ (Bi2O3+B2O3)=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)
0.7Y
0.3AlO
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
0.697Y
0.3Ce
0.003AlO
3Constant temperature is 3 hours under 1050 ℃ 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 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; 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
0.697Y
0.3Ce
0.003AlO
3/ Lu
0.7Y
0.3AlO
3The preparation of 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, a kind of Cerium aluminate lutetium yttrium sub-micrometer imaging phosphor screen of mixing is characterized in that this fluoroscopic structure is at the Lu of crystal plane direction for (010), (100) or (001)
1-zY
zAlO
3(0≤z≤1) substrate and growth flicker film (Lu thereon
1-x-yCe
yY
xAlO
3, i.e. Lu
1-x-yCe
yY
xAlO
3/ Lu
1-zY
zAlO
3(0≤x≤0.9999,0.0001≤y≤0.05,0≤z≤1).
2, the Cerium aluminate lutetium yttrium sub-micrometer imaging phosphor screen of mixing according to claim 1 is characterized in that described Lu
1-zY
zAlO
3The thickness of (0≤z≤1) substrate is the 5-30 micron, and the thickness of described flicker film is the 0.3-10 micron.
3, the fluoroscopic preparation method of Cerium aluminate lutetium yttrium sub-micrometer imaging that mixes according to claim 1 is characterized in that this phosphor screen is with the Lu of crystal plane direction for (010), (100) or (001)
1-zY
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
zY
1-zAlO
3Under the crystallization temperature of monocrystalline, and contain Lu
1-x-yCe
yY
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
yY
xAlO
3Monocrystal thin films.
4, the fluoroscopic preparation method of Cerium aluminate lutetium yttrium sub-micrometer imaging that mixes according to claim 3 is characterized in that the described Lu of containing
1-x-yCe
yY
xAlO
3The raw material proportioning of (0≤x≤0.9999,0.0001≤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 8-15mol and 1mol B
2O
3, or 10-12mol Bi
2O
3B with 1-3mol
2O
3
2. Lu
1-x-yCe
yY
xAlO
3The percentage by weight of (0≤x≤0.9999,0.0001≤y≤0.05) polycrystalline and flux is: Lu
1-x-yCe
yY
xAlO
3/ flux solution=10wt%-50wt%
5, the fluoroscopic preparation method of Cerium aluminate lutetium yttrium sub-micrometer imaging that mixes according to claim 3 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), body of heater (1) top is annealing body of heater (102), in body of heater (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), extends 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 fluoroscopic preparation method of Cerium aluminate lutetium yttrium sub-micrometer imaging that mixes according to claim 3 is characterized in that this method comprises the following steps:
＜1〉according to selected Lu
1-x-yCe
yY
xAlO
3The proportioning raw materials weighing of polycrystalline and flux is in the crucible (9) of the resistance heating liquid phase epitaxy stove 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) or (001)
1-zY
zAlO
3The substrate wafer (8) of (0≤z≤1) is inserted in the substrate clamp (7), adjusts rotary pulling bar (6), makes it to be on the coaxial position of crucible (9);
＜3〉programming rate with 100 ℃/Hr is warming up to 1050-1200 ℃, fusion polycrystal raw material Lu
1-x-yCe
yY
xAlO
3With flux PbO-B2O3 or Bi2O3-B2O3; Make it become saturated solution (10), treat all dissolvings after, 1100-1250 ℃ 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
yY
xAlO
3Under the crystallization range 900-1150 ℃ condition constant temperature 2-4 hour;
＜5〉decline rotary pulling bar (6) just in time contacts in the saturated solution (10) substrate wafer (8), and rotary pulling bar (6) is with the rotation of 100-400r/min speed, according to required growth Lu
1-x-yCe
yY
xAlO
3(0≤x≤0.9999,0.0001≤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
yY
xAlO
3(0≤x≤0.9999,0.0001≤y≤0.05) film enters upside heater (5) interval in the annealing furnace (102), the power of heater in the adjustment (5) makes its temperature after 900 ℃ of constant temperature 30-60 minutes, is cooled to room temperature with 50 ℃/hr speed then, finishes Lu
1-x-yCe
yY
xAlO
3/ Lu
1-zY
zAlO
3The preparation of (0≤x≤0.9999,0.0001≤y≤0.05,0≤z≤1) blinking screen.
7, the fluoroscopic preparation method of Cerium aluminate lutetium yttrium sub-micrometer imaging that mixes according to claim 6, it is characterized in that described step＜5〉decline rotary pulling bar (6) is before, adjust the heating power of the side heater (2) of main furnace body (101) earlier, make middle temperature thermocouple (3) be designated as 900-1150 ℃, the rotary pulling of constant temperature 1-2h, and then decline again bar (6).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102399555A (en) * | 2010-09-15 | 2012-04-04 | 海洋王照明科技股份有限公司 | Aluminate fluorescent powder and preparation method thereof |
| US8189633B2 (en) | 2005-12-13 | 2012-05-29 | General Electric Company | Polycrystalline transparent ceramic articles and method of making same |
| CN103421505A (en) * | 2013-03-25 | 2013-12-04 | 上海显恒光电科技股份有限公司 | UV single crystal fluorescence thin film grown based on liquid phase epitaxial method |
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| 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 |
| CN1176253C (en) * | 2002-07-26 | 2004-11-17 | 中国科学院上海光学精密机械研究所 | Cerium-doped lutetium yttrium aluminate lutetium aluminate composite scintillation crystal material and preparation method thereof |
-
2004
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8189633B2 (en) | 2005-12-13 | 2012-05-29 | General Electric Company | Polycrystalline transparent ceramic articles and method of making same |
| CN1982259B (en) * | 2005-12-13 | 2012-11-14 | 通用电气公司 | Polycrystalline transparent ceramic articles and method of making same |
| CN102838352A (en) * | 2005-12-13 | 2012-12-26 | 通用电气公司 | Polycrystalline transparent ceramic articles and method of making same |
| CN102399555A (en) * | 2010-09-15 | 2012-04-04 | 海洋王照明科技股份有限公司 | Aluminate fluorescent powder and preparation method thereof |
| CN102399555B (en) * | 2010-09-15 | 2013-07-24 | 海洋王照明科技股份有限公司 | Aluminate fluorescent powder and preparation method thereof |
| CN103421505A (en) * | 2013-03-25 | 2013-12-04 | 上海显恒光电科技股份有限公司 | UV single crystal fluorescence thin film grown based on liquid phase epitaxial method |
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