CN1327043C - Prepn process of Ce-doped lanthanum oxide scintillation crystal - Google Patents
Prepn process of Ce-doped lanthanum oxide scintillation crystal Download PDFInfo
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- CN1327043C CN1327043C CNB2005100633912A CN200510063391A CN1327043C CN 1327043 C CN1327043 C CN 1327043C CN B2005100633912 A CNB2005100633912 A CN B2005100633912A CN 200510063391 A CN200510063391 A CN 200510063391A CN 1327043 C CN1327043 C CN 1327043C
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- 239000013078 crystal Substances 0.000 title claims abstract description 52
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000010453 quartz Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000003708 ampul Substances 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000000155 melt Substances 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 9
- 238000012856 packing Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 5
- 230000004927 fusion Effects 0.000 claims description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000013064 chemical raw material Substances 0.000 claims description 2
- 238000002203 pretreatment Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 14
- 238000005516 engineering process Methods 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 abstract description 2
- 230000003287 optical effect Effects 0.000 abstract description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- 235000019270 ammonium chloride Nutrition 0.000 abstract 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 description 17
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 description 9
- 235000009518 sodium iodide Nutrition 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- 229910002420 LaOCl Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000009206 nuclear medicine Methods 0.000 description 2
- 230000002285 radioactive effect Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- ORCSMBGZHYTXOV-UHFFFAOYSA-N bismuth;germanium;dodecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Ge].[Ge].[Ge].[Bi].[Bi].[Bi].[Bi] ORCSMBGZHYTXOV-UHFFFAOYSA-N 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- ADOANNTYRWJJIS-UHFFFAOYSA-N lutetium silicic acid Chemical class [Lu].[Si](O)(O)(O)O ADOANNTYRWJJIS-UHFFFAOYSA-N 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000005658 nuclear physics Effects 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to a preparation method of a cerium-doped anthanum chloride scintillation single crystal, wherein the scintillation crystal has the chemical composition of La<1-x>Ce<x>Cl<3> (0.01<=x<=0.2). The present invention is characterized in that a primary raw material uses common chemical materials of La2O3, anhydrous NH4Cl and CeCl3.7H2O which are easily obtained, after the primary raw material is converted by pretreating and is melted into ingots, and is loaded in a quartz ampoule; the cerium-doped lanthanum chloride scintillation single crystal is grown by using a falling crucible method. The method uses general industrial raw materials, and has the advantage of simple production technology; the prepared crystal has the advantages of low oxygenous impurities and good optical quality.
Description
Technical field:
The present invention relates to field of crystal growth, particularly Ce-doped lanthanum oxide scintillating monocrystal chemical constitution is La
1-xCe
xCl
3, 0.01≤x≤0.3 and growth method thereof.Be specifically related to initial feed and adopt La
2O
3, anhydrous NH
4Cl and CeCl
37H
2The general chemical raw material that O is easy to obtain after also melting becomes piece through the pre-treatment conversion, in the quartz ampoule bottle of packing into, adopts falling crucible method to carry out the growth of Ce-doped lanthanum oxide scintillation crystal.
Background technology:
Scintillation crystal is widely used in surveying high energy particles such as gamma rays, X ray, Millikan's rays and electronics, neutron.Scintillation crystal can be launched light pulse under radioactive rays or particle effect, this light pulse sees through behind the crystal by photomultiplier, after receiving, photoelectric devices such as avalanche photodide are transformed into the electric impulse signal that has amplified, people write down and store this electric impulse signal, thereby realize the detection to radioactive rays.Scintillation crystal can be widely used in industrial online detection, oil well logging, image nuclear medicine (PET, CT) and fields such as high energy physics and nuclear physics research.
What be most widely used in the scintillation crystal wants Shuo Can sodium iodide (NaI (Tl)) crystal, and it is to find in 1948, still occupies main market so far.This mainly is that one of its main drawback is that luminescence decay time is slower, is unfavorable for high counting rate work because it has the energy resolution of high photoyield and appropriateness.Bismuth germanium oxide (BGO) scintillation crystal is owing to have bigger density (ρ=7.13g/cm3) and effective atom coefficient (Z
Eff=74), obtained application at high energy physics and nuclear medicine facility fields such as (PET), but grown (300ns) its fall time, drawbacks limit such as photoyield little (be equivalent to NaI (Tl) 7～10%) its range of application.
Since the nineties, the high temperature scintillation crystals such as silicic acid lutetium series of mixing cerium are developed, however this crystalloid fusing point very high (about 2200 ℃), the manufacturing process difficulty, thereby the crystal price is more expensive.
Recently, it is found that the lanthanum chloride crystal (Ce:LaCl that mixes cerium
3) be the outstanding inorganic scintillation crystal of a kind of performance.LaCl
3Crystal has six crystallographic system UCl
3Structure, density are 3.9g/cm
3, this compound is 860 ℃ of following congruent meltings, thereby is suitable for various growing technologies based on melt and carries out crystal growth.This crystal have the output of very high light (50,000 photons/MeV) and fast fall time (～20ns).And it has very high energy resolution (for 662keV γ photon radiation, its energy resolution (FWHM) is 3.2%), and very high temporal resolution.Referring to: Nuclear Instruments and Methods in PhysicsResearchA the 505th volume 2003,76-81 page or leaf.
Formerly in the technology, Ce-doped lanthanum oxide scintillation crystal (Ce:LaCl
3) crystal growing process in, generally be to adopt anhydrous super dried LaCl
3With powder CeCl
3Be raw material, the silica tube of packing into after this raw material mixes in molar ratio vacuumizes tube sealing again, and then the material pipe that will seal is put into bridgman furnace and carried out crystal growth.Referring to U.S.Pat.No:20040238747A1.
Technology growth Ce:LaCl formerly
3Scintillation crystal has following shortcoming: anhydrous LaCl
3, CeCl
3The raw material powder surfactivity is very big, hygroscopic property is extremely strong, therefore the batch mixes of raw material and the process of tubulation seals all must be carried out under super dry atmosphere, especially in the process that vacuumizes envelope material pipe, because of the operating time longer, the material pipe must heat, and is careless slightly, very easily causes the raw material part moisture absorption or heating to cause LaCl
3Hydrolysis reaction generate LaOCl impurity, LaOCl becomes infusible La in follow-up high temperature melting process
2O
3, be mingled with micro-La
2O
3LaCl
3The crystal that melt growth goes out ftractures easily, causes lattice defect to increase to I haven't seen you for ages, downgrade.
In addition, technology growth Ce:LaCl formerly
3The anhydrous LaCl of commodity raw material that crystal adopted
3With anhydrous CeCl
3Often contain a certain amount of oxygen in the powder.In order to obtain fine LaCl
3Crystal requires in the raw material foreign matter content less than 0.1%, referring to U.S.Pat.No:20040238747A1, needs that for this reason raw material is carried out vacuum-evaporation and purifies, and this has just increased the complicacy and the production cost of technology greatly.
Summary of the invention:
The objective of the invention is to overcome the shortcoming of technology formerly, a kind of Ce:LaCl is provided
3The preparation method of scintillation crystal, this method adopts the general industry raw material, and production technique is simple, and prepared crystal oxygenate impurity is lower, has optical quality preferably.
Key of the present invention is formally to pack into before quartzy material pipe carries out crystal growth at required muriate raw material, is fused into ingot in advance, becomes bigger polycrystalline piece, significantly reduced in the charging tube sealing process since the excessive material that causes of material specific surface area to O
2, H
2The absorption of detrimental impurity such as O.Key of the present invention is that also required anhydrous chlorides of rase raw material is that real-world effectiveness obtains and is unlikely to be hydrolyzed with oxidized all the time under the HCl atmosphere protection till being fused into ingot.Technical solution of the present invention is as follows:
The present invention prepares LaCl
3The crystalline process mainly is divided into three phases:
First stage is the feedstock conversion stage, respectively with La
2O
3Be converted into anhydrous LaCl
3, with CeCl
37H
2O is converted into anhydrous CeCL
3,, adopt the excessive proportioning NH of super large in conversion process
4Cl participates in reaction, and adopts the long-time reaction process of low temperature.The main chemical reactions process that fs relates to is as follows:
10NH
4Cl+La
2O
3→2(NH
4)
2[LaCl
5]+6NH
3+3H
2O (1)
2NH
4Cl+CeCl
3·7H
2O→(NH
4)
2[CeCl
5]+7H
2O (2)
(NH
4)
2[LaCl
5]→LaCl
3+2NH
4Cl (3)
(NH
4)
2[CeCl
5]→CeCl
3+2NH
4Cl (4)
Subordinate phase is the melt tube sealing stage, with above-mentioned NH
4ClLaCl
3And NH
4ClCeCl
3Pack into after powder mixes by a certain percentage in silica tube fusing and be cooled to ingot rapidly.Crystal ingot is smashed quartzy material pipe of back dress and sealing.
Phase III is put into vertically two warm area bridgman furnaces for the long brilliant stage with above-mentioned material pipe, adopts material pipe descent method for growing crystal.
Concrete step of preparation process is as follows:
＜1〉purity is greater than 99.98% La
2O
3, enter in the vacuum drying oven 200 ℃-250 ℃ roasting 10-30 hour;
＜2〉by above-mentioned chemical equation＜1〉left side two component molar weights are with NH
4The big extra proportion batching of Cl: concrete mole proportioning is as follows:
La
2O
3∶NH
4Cl＝1∶(15～25)；
＜3〉with step＜2〉batching to put into stoving oven be under 150 ℃-300 ℃ in temperature, in air, or in the nitrogen gas stream roasting 20-60 hour.Calcination vessel is quartz curette or the alumina-ceramic cup that lid is arranged;
＜4〉with CeCl
37H
2O and NH
4Cl prepares burden in following ratio, and concrete mol ratio proportioning is as follows:
CeCl
3·7H
2O∶NH
4Cl＝1∶(8～15)；
＜5〉above-mentioned batching is put into quartz boat and vacuumize drying at the horizontal pipe stove, drying temperature is 250 ℃-420 ℃, and be 20-60 hour time of drying, and system outlet vacuum tightness generally maintains 10Pa-100Pa;
＜6〉with above-mentioned steps＜3〉and step＜5 product in glove box, mix by a certain percentage, make LaCl
3With CeCl
3Mol ratio be 1: pack into and melt in the melt pipe in (0.02～0.3), the material powder that mixes.The melt pipe is the quartz container of design in small direct draught work, and system's gauge pressure is 0.1～5kPa in the melt process;
＜7〉material is warming up to 900 ℃-930 ℃ in the melt pipe, is incubated i.e. cooling fast after 1-2 hour, and the time that generally is cooled to 200 ℃ should be above 6-10 hour;
＜8〉crystal ingot that the fusion cooling is obtained is broken into the particle that granularity is 5～10mm in vacuum glove box, in the quartz ampoule bottle of packing into.Ampoule is evacuated to 10
-3Seal behind the Pa;
＜9〉the above-mentioned ampoule of sealing is put into crucible at two warm area bridgman furnace growing crystals, dropping speed of the crucible 1～5mm/h, speed of rotation is 0.5～5rpm.
Below by embodiment the present invention is specifically described:
Embodiment 1: preparation LaCl
3(3%CeCl
3) Ce-doped lanthanum oxide scintillation crystal
Concrete step of preparation process is as follows:
＜1〉purity is greater than 99.98% La
2O
3, enter in the vacuum drying oven 200 ℃-250 ℃ roasting 10-30 hour;
＜2〉press above-mentioned chemical equation (1) left side two component molar weights with NH
4The big extra proportion batching of Cl: concrete mole proportioning is as follows:
La
2O
3∶NH
4Cl＝1∶15；
＜3〉with step＜2〉batching to put into stoving oven be under 150 ℃-300 ℃ in temperature, in air, or in the nitrogen gas stream roasting 20-60 hour.Calcination vessel is quartz curette or the alumina-ceramic cup that lid is arranged;
＜4〉with CeCl
37H
2O and NH
4Cl prepares burden in following ratio, and concrete mol ratio proportioning is as follows:
CeCl
3·7H
2O∶NH
4Cl＝1∶8；
＜5〉above-mentioned batching is put into quartz boat and is vacuumized drying at the horizontal pipe stove, and drying temperature is 250 ℃-420 ℃, and be 20-60 hour time of drying, and system outlet vacuum tightness generally maintains 10Pa-100Pa;
＜6〉with above-mentioned steps＜3〉and step＜5 product in glove box, mix by a certain percentage, make LaCl
3With CeCl
3Mol ratio be 1: pack into and melt in the melt pipe in (0.02～0.3), the material powder that mixes.The melt pipe is the quartz container of design in small direct draught work, and system's gauge pressure is 0.1～5kPa in the melt process;
＜7〉material is warming up to 900 ℃-930 ℃ in the melt pipe, is incubated i.e. cooling fast after 1-2 hour, and the time that generally is cooled to 200 ℃ should be above 6-10 hour;
＜8〉crystal ingot that the fusion cooling is obtained is broken into the particle that granularity is 5～10mm in vacuum glove box, in the quartz ampoule bottle of packing into.Ampoule is evacuated to 10
-3Seal behind the Pa;
＜9〉the above-mentioned ampoule of sealing is put into crucible at two warm area bridgman furnace growing crystals, dropping speed of the crucible 1～5mm/h, speed of rotation is 0.5～5rpm.Can obtain perfect crystalline at last, water white crystal.
Embodiment 2: preparation LaCl
3(10%CeCl
3) Ce-doped lanthanum oxide scintillation crystal
Concrete step of preparation process is as follows:
＜1〉purity is greater than 99.98% La
2O
3, enter in the vacuum drying oven 200 ℃-250 ℃ roasting 10-30 hour;
＜2〉by above-mentioned chemical equation＜1〉left side two component molar weights are with NH
4The big extra proportion batching of Cl: concrete mole proportioning is as follows:
La
2O
3∶NH
4Cl＝1∶19；
＜3〉with step＜2〉batching to put into stoving oven be under 150 ℃-300 ℃ in temperature, in air, or in the nitrogen gas stream roasting 20-60 hour.Calcination vessel is quartz curette or the alumina-ceramic cup that lid is arranged;
＜4〉with CeCl
37H
2O and NH
4Cl prepares burden in following ratio, and concrete mol ratio proportioning is as follows:
CeCl
3·7H
2O∶NH
4Cl＝1∶10；
＜5〉above-mentioned batching is put into quartz boat and vacuumize drying at the horizontal pipe stove, drying temperature is 250 ℃-420 ℃, and be 20-60 hour time of drying, and system outlet vacuum tightness generally maintains 10Pa-100Pa;
＜6〉with above-mentioned steps＜3〉and step＜5 product in glove box, mix by a certain percentage, make LaCl
3With CeCl
3Mol ratio be 1: pack into and melt in the melt pipe in (0.02～0.3), the material powder that mixes.The melt pipe is the quartz container of design in small direct draught work, and system's gauge pressure is 0.1～5kPa in the melt process;
＜7〉be warming up to 900 ℃-930 ℃ in the melt pipe, be incubated i.e. cooling fast after 1-2 hour, the time that generally is cooled to 200 ℃ should be above 6-10 hour;
＜8〉crystal ingot that the fusion cooling is obtained is broken into the particle that granularity is 5～10mm in vacuum glove box, in the quartz ampoule bottle of packing into.Ampoule is evacuated to 10
-3Seal behind the Pa;
＜9〉the above-mentioned ampoule of sealing is put into crucible at two warm area bridgman furnace growing crystals, dropping speed of the crucible 1～5mm/h, speed of rotation is 0.5～5rpm.Can obtain perfect crystalline at last, water white crystal.
Embodiment 3: preparation LaCl
3(3%CeCl
3) Ce-doped lanthanum oxide scintillation crystal
Concrete step of preparation process is as follows:
＜1〉purity is greater than 99.98% La
2O
3, enter in the vacuum drying oven 200 ℃-250 ℃ roasting 10-30 hour;
＜2〉state chemical equation＜1〉left side two component molar weights are with NH
4The big extra proportion batching of Cl: concrete mole proportioning is as follows:
La
2O
3∶NH
4Cl＝1∶22；
＜3〉with step＜2〉batching to put into stoving oven be under 150 ℃-300 ℃ in temperature, in air, or in the nitrogen gas stream roasting 20-60 hour.Calcination vessel is quartz curette or the alumina-ceramic cup that lid is arranged;
＜4〉with CeCl
37H
2O and NH
4Cl prepares burden in following ratio, and concrete mol ratio proportioning is as follows:
CeCl
3·7H
2O∶NH
4Cl＝1∶15；
＜5〉above-mentioned batching is put into quartz boat and vacuumize drying at the horizontal pipe stove, drying temperature is 250 ℃-420 ℃, and be 20-60 hour time of drying, and system outlet vacuum tightness generally maintains 10Pa-100Pa;
＜6〉with above-mentioned steps＜3〉and step＜5 product in glove box, mix by a certain percentage, make LaCl
3With CeCl
3Mol ratio be 1: pack into and melt in the melt pipe in (0.02～0.3), the material powder that mixes.The melt pipe is the quartz container of design in small direct draught work, and system's gauge pressure is 0.1～5kPa in the melt process;
＜7〉material is warming up to 900 ℃-930 ℃ in the melt pipe, is incubated i.e. cooling fast after 1-2 hour, and the time that generally is cooled to 200 ℃ should be above 6-10 hour;
＜8〉crystal ingot that the fusion cooling is obtained is broken into the particle that granularity is 5～10mm in vacuum glove box, in the quartz ampoule bottle of packing into.Ampoule is evacuated to 10
-3Seal behind the Pa;
＜9〉the above-mentioned ampoule of sealing is put into crucible at two warm area bridgman furnace growing crystals, dropping speed of the crucible 1～5mm/h, speed of rotation is 0.5～5rpm.Can obtain perfect crystalline at last, water white crystal.
Claims (4)
1. the preparation method of a Ce-doped lanthanum oxide scintillating monocrystal, the chemical constitution of this scintillation crystal is La
1-xCe
xCl
3, 0.01≤x≤0.3; It is characterized in that initial feed adopts La
2O
3, anhydrous NH
4Cl and CeCl
37H
2The general chemical raw material that O is easy to obtain after also melting becomes piece through the pre-treatment conversion, in the quartz ampoule bottle of packing into, adopts falling crucible method to carry out the growth of Ce-doped lanthanum oxide scintillation crystal.
2. the preparation method of Ce-doped lanthanum oxide scintillating monocrystal according to claim 1 is characterized in that present method comprises the following steps:
＜1〉purity is greater than 99.98% La
2O
3, enter in the vacuum drying oven 200 ℃-250 ℃ roasting 10-30 hour;
＜2〉press above-mentioned chemical equation (1) left side two component molar weights with NH
4The big extra proportion batching of Cl: concrete mole proportioning is as follows:
La
2O
3∶NH
4Cl＝1∶(15～25)；
＜3〉with step＜2〉batching to put into stoving oven be under 150 ℃-300 ℃ in temperature, in air or in the nitrogen gas stream roasting 20-60 hour; Calcination vessel is quartz curette or the alumina-ceramic cup that lid is arranged;
＜4〉with CeCl
37H
2O and NH
4Cl prepares burden in following ratio, and concrete mol ratio proportioning is as follows:
CeCl
3·7H
2O∶NH
4Cl＝1∶(8～15)；
＜5〉above-mentioned batching is put into quartz boat and vacuumize drying at the horizontal pipe stove, drying temperature is 250 ℃-420 ℃, and be 20-60 hour time of drying, and system outlet vacuum tightness generally maintains 10Pa-100Pa;
＜6〉with above-mentioned steps＜3〉and step＜5 product in glove box, mix by a certain percentage, make LaCl
3With CeCl
3Mol ratio be 1: pack into and melt in the melt pipe in (0.02～0.3), the material powder that mixes; The melt pipe is the quartz container of design in small direct draught work, and system's gauge pressure is 0.1～5kPa in the melt process;
＜7〉material is warming up to 900 ℃-930 ℃ in the melt pipe, is incubated i.e. cooling fast after 1-2 hour, and the time that generally is cooled to 200 ℃ should be above 6-10 hour;
＜8〉crystal ingot that the fusion cooling is obtained is broken into the particle that granularity is 5～10mm in vacuum glove box, in the quartz ampoule bottle of packing into; Ampoule is evacuated to 10
-3Seal behind the pa;
＜9〉the above-mentioned ampoule of sealing is put into crucible at two warm area bridgman furnace growing crystals, dropping speed of the crucible 1～5mm/h, speed of rotation is 0.5～5rpm.
3. the preparation method of Ce-doped lanthanum oxide scintillating monocrystal according to claim 2 is characterized in that step＜6〉described melt becomes the ingot process to carry out containing under the HCl atmosphere.
4. the preparation method of Ce-doped lanthanum oxide scintillating monocrystal according to claim 2 is characterized in that step＜9〉in used crucible can use quartz material, also can make of alumina material.
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|---|---|---|---|
| CNB2005100633912A CN1327043C (en) | 2005-04-12 | 2005-04-12 | Prepn process of Ce-doped lanthanum oxide scintillation crystal |
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|---|---|---|---|
| CNB2005100633912A CN1327043C (en) | 2005-04-12 | 2005-04-12 | Prepn process of Ce-doped lanthanum oxide scintillation crystal |
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| Publication Number | Publication Date |
|---|---|
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| CN1327043C true CN1327043C (en) | 2007-07-18 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2426694C1 (en) * | 2010-02-15 | 2011-08-20 | Общество С Ограниченной Ответственностью "Сцинтилляционные Технологии Радиационного Контроля" | Inorganic scintillation material, crystalline scintillator and radiation detector |
| WO2012066425A2 (en) | 2010-11-16 | 2012-05-24 | Saint-Gobain Cristaux Et Detecteurs | Scintillation compound including a rare earth element and a process of forming the same |
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