CN105986320A - Sc/Ce-codoped lutetium silicate and lutetium yttrium silicate crystals and melt-process growth method thereof - Google Patents
Sc/Ce-codoped lutetium silicate and lutetium yttrium silicate crystals and melt-process growth method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/34—Silicates
Abstract
The invention discloses Sc/Ce-codoped lutetium silicate and lutetium yttrium silicate crystals and a melt-process growth method thereof. The molecular formulae are Sc[2x]Ce[2y]Lu2[(1-x-y)]SiO[5] and Sc[2x]Ce[2y]Y[2z]Lu[2(1-x-y-z)]SiO[5]. The melt-process growth method comprises the following steps: as for the Sc[2x]Ce[2y]Lu2[(1-x-y)]SiO[5], proportionally preparing Sc2O3, CeO2, Lu2O3 and SiO2, sufficiently mixing, carrying out press forming, and carrying out high-temperature sintering to obtain a crystal growth initial raw material; or as for the Sc[2x]Ce[2y]Y[2z]Lu[2(1-x-y-z)]SiO[5], proportionally preparing Sc2O3, CeO2, Y2O3, Lu2O3 and SiO2, sufficiently mixing, carrying out press forming, and carrying out high-temperature sintering to obtain a crystal growth initial raw material; and heating to melt the growth initial raw material, and growing by a dip coating process or crucible descent process to obtain the scintillator monocrystals.
Description
Technical field
The present invention relates to the high-energy ray such as high-energy physics, nuclear medicine or high energy particle detection required for inorganic
Scintillator and field of crystal growth, the silicic acid lutecium of specially two kinds Sc, Ce codopes, yttrium luetcium silicate crystal and
Melt-method growth process.
Background technology
The fast decay of luminescence of scintillator and high density characteristic are modern key indexs required by nuclear medicine.Hurry up
Decay of luminescence is conducive to detection and differentiates physical event, reaches to screen, detect the purpose of high energy particle；Cure at core
Studying in picture, fast decay scintillator will be greatly shortened imaging time, improve and check efficiency.Meanwhile, high density is dodged
Bright body has high stopping power and short irradiation length, and under identical detectivity requires, this will subtract significantly
The little scintillator detection array volume being made up of thousands of, tens thousand of or even more than 100,000 crystal, and peripheral accordingly
Equipment volume, significantly reduces construction cost.In large-scale nuclear medicine PET system, whole detector by 8～
11 detection ring compositions, each detection ring is made up of 512 detection components and parts again, and required crystal element is 4000
More than root, therefore the high density scintillator of short irradiation length is conducive to the miniaturization of instrument, improves detection simultaneously
Sensitivity and image resolution ratio.
In the inorganic fast scintillator reported, a class is the luminescence of substrate itself, such as CuI, BaF2、PbWO4。
Current this kind of material is the fastest with the luminescence decay time of CuI, has reached 90ps, but this crystal growth is difficult,
It is application and the bottleneck of research；BaF2195,220, the fluorescence decay time of 310nm be respectively 0.87,
0.88 and 600ns, but its density is only 4.88g/cm3, photoyield, less than the 1/5 of BGO, in use needs
KCsTe or the Rb-Te photomultiplier tube of speciality to be passed through filters slow component to obtain being bordering on pure fast composition letter
Number；PbWO4Fluorescence decay time be 15ns, but photoyield only has about the 3% of BGO.
An other inorganic fast scintillator of class is with rare earth ion Ce3+、Pr3+、Nd3+As activator or work itself
For a part for substrate, utilize Ce3+、Pr3+、Nd3+5d → 4f parity allowed transition obtain fast decay and send out
Light, luminescence decay time is about at 10～100ns scopes, the fast scintillator being activation ion with Ce the most again
Research and development most species.These materials include that halogenide, bromide and fluoride are (such as Ce:LaCl3、
Ce:LaBr3、Ce:LaI3、Ce:LuCl3、Ce:LuBr3、Ce:LuI3、CeF3、K2CeBr5、K2CeCl5、
Cs2CeBr5)、Pr:KY3F10), aluminium garnet X3Al5O12(X=Y, Lu, Y/Lu, as Ce:YAG, Ce:LuAG,
Pr:LuAG), aluminum perovskite oxide Ce:XAlO3The silicate crystal of (X:=L, Y, Y/Lu), Ce doping
(Gd2SiO5:Ce(GSO:Ce)、Lu2SiO5:Ce(LSO:Ce)、Y2SiO5:Ce(YSO:Ce)、
Lu2Si2O7:Ce(LPS:Ce)、Y2Si2O7:Ce(YPS:Ce)、Gd2-xYxSiO5:Ce(GYSO:Ce)、
Lu2-xYxSiO5:Ce(LYSO:Ce))、Ce:XHfO3(X=Sr, Ba) etc..
In these crystal, Ce:XHfO3Although the high (Ce:BaHfO of density3Density be 8.5g/cm3, cube
SrHfO3Density be 7.492g/cm3), but their fusing point is more than 3000K, and single crystal preparation is difficult, at present
People are directed generally to study their crystalline ceramics technology of preparing.But it is expensive and the Hf raw material of rareness is also this
One obstacle of class materials application.In remaining crystal, density is more than 7g/cm3Only have LSO:Ce,
LuAlO3: Ce, and LYSO:Ce, Lu of obtaining that both materials are substrate incorporation Y1-xYxAlO3:Ce。
In nuclear medicine, generally to density more than 7g/cm3High density scintillator LSO:Ce (Lu2SiO5: Ce) and
LuAP:Ce(LuAlO3: Ce) promise well, and by LSO:Ce, LYAP:Ce, LYSO:Ce
(Lu0.6Y1.4SiO5: Ce), mixing silicic acid lutecium MLS, GSO:Ce (Gd2SiO5:Ce)、GSO:Zr:Ce
(Gd2SiO5:Ce:Zr)、LGSO:Ce(Lu0.2Gd1.8SiO5:Ce)、LaBr3:Ce、LaCl3:Ce、BGO、
CdWO4Performance comparison research show, the performance of LSO:Ce is optimal, is significantly better than BGO.But LSO:Ce
Shortcoming be containing176Lu, has stronger Background radiation, and energy resolution is also not as GSO:Ce.Therefore, Y
Substitute part Gd in Ce:LSO crystal and can reduce Lu background, reduce the background of LSO, and cost of material
Decline, but the advantage that the scintillator of Ce:LSO can be kept.Therefore, Ce:LSO, Ce:LYSO
Become the scintillator that the combination property of development PET imaging is best.
The fluorescence lifetime of Ce:LSO, Ce:LYSO is about at 30ns, and experiment finds, if, in both scintillators
Mix Sc, fluorescence lifetime can be shortened to about 20s, i.e. fluorescence lifetime can shorten about 30%, for some
The ray or the high energy particle field of detecting that need fast attenuation high-efficiency obviously have great importance.
Summary of the invention
It is an object of the invention to provide the silicic acid lutecium of two kinds of Sc, Ce codopes, yttrium luetcium silicate crystal and melt thereof
Method growing method, the bi-material of preparation is the scintillator monocrystalline of function admirable, becomes in high-energy physics, nuclear medicine
There is important application prospect in the fields such as picture.
For achieving the above object, the technical solution used in the present invention is as follows:
The silicic acid lutecium of Sc, Ce codope, yttrium luetcium silicate crystal, it is characterised in that its molecular formula can represent respectively
For Sc2xCe2yLu2(1-x-y)SiO5And Sc2xCe2yY2zLu2(1-x-y-z)SiO5, wherein, the span of x, y, z
For: 0 < x < 1,0 < y < 1,0 < z < 1, and x, y meet 0 < x+y < 1, x, y, z meets 0 < x+y+z < 1.
The silicic acid lutecium of described Sc, Ce codope, yttrium luetcium silicate crystal melt-method growth process as follows:
(1) for Sc2xCe2yLu2(1-x-y)SiO5, use Sc2O3、CeO2、Lu2O3、SiO2As raw material,
Dispensing is carried out by following chemical equation (Eq-1),
(Eq-1)
The Sc obtained will be weighed in (Eq-1) reaction equation ratio2O3、CeO2、Lu2O3、SiO2Mixture abundant
Mix homogeneously, after being pressed into cake or cylindrical block, calcines 24-200 hour at 900-1300 DEG C
Solid state reaction is occurred to obtain the polycrystal raw material needed for growth crystal；Or weigh in (Eq-1) reaction equation ratio and obtain
Sc2O3、CeO2、Lu2O3、SiO2After mixture is pressed into cake or cylindrical block, burn without extra
Knot is directly used as crystal growth initial feed；
(2) for Sc2xCe2yY2zLu2(1-x-y-z)SiO5, to using Sc2O3、CeO2、Y2O3、Lu2O3、SiO2
As raw material, carry out dispensing by following chemical equation (Eq-2),
(Eq-2)
To weigh by (Eq-2) reaction equation and obtain Sc2O3、CeO2、Y2O3、Lu2O3、SiO2Mixture is the most mixed
Close uniformly, after being pressed into cake or cylindrical block, calcine at 900-1300 DEG C 24-200 hour and send out
Raw solid state reaction obtains the polycrystal raw material needed for growth crystal；Or weigh by (Eq-2) reaction equation and obtain Sc2O3、
CeO2、Y2O3、Lu2O3、SiO2After mixture is pressed into cake or cylindrical block, straight without extra sintering
Connect as crystal growth initial feed；
(3) the crystal growth initial feed of above-mentioned preparation is put into growth iridium crucible, molybdenum crucible or tungsten crucible,
Heated by sensing or resistance heats and fully melts, it is thus achieved that crystal growth melt；Then melt method crystal is used
Growth technique-czochralski method, Bridgman-Stockbarger method, temperature ladder method, heat-exchanging method, kyropoulos, top-seeded solution growth, help
Flux growing method, or micro-glass tube down-drawing (μ-PD) grows, and growth atmosphere can be air atmosphere, oxygen
Activating QI atmosphere, argon gas atmosphere, nitrogen atmosphere, CO2Atmosphere or CO atmosphere.
Sc2xCe2yLu2(1-x-y)SiO5And Sc2xCe2yY2zLu2(1-x-y-z)SiO5Generally use seed crystal oriented growth, seed
Brilliant available Sc2xCe2yLu2(1-x-y)SiO5、Sc2xCe2yY2zLu2(1-x-y-z)SiO5Monocrystalline Lu2SiO5Monocrystalline or
Y2uLu2(1-u)SiO5(0<u<1) monocrystalline, seed crystal direction is<100>,<010>or<001>direction；Also can not adopt
Grow with seed crystal diameter.
At Sc2xCe2yLu2(1-x-y)SiO5Or Sc2xCe2yY2zLu2(1-x-y-z)SiO5In the growth raw material preparation of crystal,
Raw materials used Sc2O3、CeO2、Y2O3、Lu2O3、SiO2Corresponding Sc, Ce, Y, Lu, Si can be used
Other compound replace, Material synthesis method includes high temperature solid state reaction, liquid phase synthesis, gas-phase synthesizing method,
But need to meet and can ultimately form compound Sc by chemical reaction2xCe2yLu2(1-x-y)SiO5With
Sc2xCe2yY2zLu2(1-x-y-z)SiO5This condition.
Beneficial effect
The present invention, by the Sc that adulterates in Ce:LSO, Ce:LYSO, accelerates their Ce effectively3+Luminous
Life-span, be conducive to improve detection temporal resolution.Such as, for Lu1.988Ce0.012SiO5, Ce3+Send out
Light decay to 34ns, and for the Lu of Sc doping1.388Ce0.012Sc0.6SiO5, Ce3+The time of decay of luminescence
It is only 23ns, accelerates 30%.Bi-material prepared by the inventive method is the scintillator monocrystalline of function admirable,
Important application prospect is had in the field such as high-energy physics, nuclear medicine.
Accompanying drawing explanation
Fig. 1 is Sc2xCe2yLu2(1-x-y)SiO5Life-span with the change curve of Sc doping content, give difference
The fluorescence decay curve of Ce:LSO under Sc doping content, along with Sc concentration increases to 0.6,
Sc2xCe2yLu2(1-x-y)SiO5Fluorescence lifetime decay to 23ns.
Detailed description of the invention
Embodiment 1 grows Sc2xCe2yLu2(1-x-y)SiO5Crystal
Take x=0.1, y=0.0015 and grow Sc2xCe2yLu2(1-x-y)SiO5Crystal, if former needed for crystals growth
Material is 100g, then crystal growth method by melt method is as follows:
(1) Sc is used2O3、CeO2、Lu2O3、SiO2As raw material, by chemical equation: Carry out
Dispensing, takes 3.19g Sc in this ratio nominal2O3、0.12g CeO2、82.78g Lu2O3、13.91g SiO2Fill
Divide mix homogeneously, obtain ingredients mixture；
(2) just mixture is pressed into round pie, calcines 96 hours, it is thus achieved that crystal growth is initial at 1300 DEG C
Raw material；
(3) crystal growth initial feed is put into growth iridium crucible, utilizes JGD600 type single crystal growing furnace system,
By Frequency Induction Heating and fully melt, it is thus achieved that crystal growth initial melt；Then use czochralski method crystal raw
Long technique, with the silicic acid lutecium monocrystalline in<001>direction for seed crystal oriented growth, it is thus achieved that<001>direction growth
Sc2xCe2yLu2(1-x-y)SiO5Monocrystalline.
Embodiment 2 grows Sc2xCe2yY2zLu2(1-x-y-z)SiO5Crystal
Taking x=0.1, y=0.0015, z=0.2 grow Sc2xCe2yY2zLu2(1-x-y-z)SiO5Crystal, if crystals growth
Required raw material is 100g, then crystal growth method by melt method is as follows:
(1) Sc is used2O3、CeO2、Lu2O3、SiO2As raw material, by chemical equation: Carry out dispensing, take 3.50g Sc in this ratio nominal2O3、0.13g CeO2、69.66g Lu2O3、
11.46g Y2O3、15.24g SiO2It is sufficiently mixed uniformly, obtains ingredients mixture；
(2) just mixture is pressed into round pie, calcines 96 hours, it is thus achieved that crystal growth is initial at 1300 DEG C
Raw material；
(3) crystal growth initial feed is put into growth iridium crucible, utilize JGD600 type single crystal growing furnace system, pass through
Frequency Induction Heating also fully melts, it is thus achieved that crystal growth initial melt；Then method of crystal growth by crystal pulling work is used
Skill, with the silicic acid lutecium monocrystalline in<001>direction for seed crystal oriented growth, it is thus achieved that<001>direction growth
Sc2xCe2yY2zLu2(1-x-y-z)SiO5Monocrystalline.
Claims (5)
- The silicic acid lutecium of 1.Sc, Ce codope, yttrium luetcium silicate crystal, it is characterised in that its molecular formula table respectively It is shown as Sc2xCe2yLu2(1-x-y)SiO5And Sc2xCe2yY2zLu2(1-x-y-z)SiO5, wherein, the value model of x, y, z Enclose for: 0 < x < 1,0 < y < 1,0 < z < 1, and x, y meet 0 < x+y < 1, x, y, z meets 0 < x+y+ z<1。
- 2. the melt method life of the silicic acid lutecium of Sc, Ce codope as claimed in claim 1, yttrium luetcium silicate crystal Long method, it is characterised in that include following operation:(1) for Sc2xCe2yLu2(1-x-y)SiO5, use Sc2O3、CeO2、Lu2O3、SiO2As raw material, Dispensing is carried out by following chemical equation (Eq-1),The Sc obtained will be weighed in (Eq-1) reaction equation ratio2O3、CeO2、Lu2O3、SiO2Mixture abundant Mix homogeneously, after being pressed into cake or cylindrical block, calcines 24-200 hour at 900-1300 DEG C Solid state reaction is occurred to obtain the polycrystal raw material needed for growth crystal；Or weigh in (Eq-1) reaction equation ratio and obtain Sc2O3、CeO2、Lu2O3、SiO2After mixture is pressed into cake or cylindrical block, burn without extra Knot is directly used as crystal growth initial feed；(2) for Sc2xCe2yY2zLu2(1-x-y-z)SiO5, to using Sc2O3、CeO2、Y2O3、Lu2O3、 SiO2As raw material, carry out dispensing by following chemical equation (Eq-2),To weigh by (Eq-2) reaction equation and obtain Sc2O3、CeO2、Y2O3、Lu2O3、SiO2Mixture is abundant Mix homogeneously, after being pressed into cake or cylindrical block, calcines 24-200 hour at 900-1300 DEG C Solid state reaction is occurred to obtain the polycrystal raw material needed for growth crystal；Or weigh by (Eq-2) reaction equation and obtain Sc2O3、CeO2、Y2O3、Lu2O3、SiO2After mixture is pressed into cake or cylindrical block, without volume Externally sintered it is directly used as crystal growth initial feed；(3) the crystal growth initial feed of above-mentioned preparation is respectively put into growth iridium crucible, molybdenum crucible or tungsten crucible In, heated by sensing or resistance heats and fully melts, it is thus achieved that crystal growth melt；Then melt method is used Crystal growth technique-czochralski method, Bridgman-Stockbarger method, temperature ladder method, heat-exchanging method, kyropoulos, top-seeded solution growth, Flux growing method, micro-glass tube down-drawing (μ-PD) grow.
- The silicic acid lutecium of Sc the most according to claim 2, Ce codope, the melt method of yttrium luetcium silicate crystal Growing method, it is characterised in that described growth atmosphere can be air atmosphere, oxidizing atmosphere, argon gas atmosphere, Nitrogen atmosphere, CO2Atmosphere or CO atmosphere.
- The silicic acid lutecium of Sc the most according to claim 2, Ce codope, the melt method life of yttrium luetcium silicate crystal Long method, it is characterised in that: described crystal growth method by melt includes not using seeded growth and employing seed crystal Oriented growth；For using seed crystal oriented growth, seed crystal is Sc2xCe2yLu2(1-x-y)SiO5Or Sc2xCe2yY2zLu2(1-x-y-z)SiO5Monocrystalline, or use silicic acid lutecium Lu2SiO5Monocrystalline, Y2uLu2(1-u)SiO5(0<u<1) monocrystalline, seed crystal direction is<100>,<010>or<001>direction.
- The silicic acid lutecium of Sc the most according to claim 2, Ce codope, the melt method for growing of yttrium luetcium silicate crystal Method, it is characterised in that in described dispensing, raw materials used Sc2O3、CeO2、Y2O3、Lu2O3、SiO2, Other compound that can use corresponding Sc, Ce, Y, Lu, Si replaces, and Material synthesis method includes high temperature Solid state reaction, liquid phase synthesis, gas-phase synthesizing method, but need to meet and can ultimately form chemical combination by chemical reaction Thing Sc2xCe2yLu2(1-x-y)SiO5And Sc2xCe2yY2zLu2(1-x-y-z)SiO5This condition.
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| CN111910254A (en) * | 2020-08-04 | 2020-11-10 | 南昌大学 | Cerium-doped and erbium-doped ytterbium silicate scintillation crystal and preparation method thereof |
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