CN102534802A - Process for modifying lead tungstate crystal by utilizing diffusion method - Google Patents
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- CN102534802A CN102534802A CN2011104259793A CN201110425979A CN102534802A CN 102534802 A CN102534802 A CN 102534802A CN 2011104259793 A CN2011104259793 A CN 2011104259793A CN 201110425979 A CN201110425979 A CN 201110425979A CN 102534802 A CN102534802 A CN 102534802A
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Abstract
The invention discloses a process for modifying a lead tungstate crystal by utilizing a diffusion method, which comprises the steps of (1) utilizing lead oxide (PbO) powder and tungsten trioxide (WO3) powder to serve as raw materials, performing accurate dosing according to the molar ratio of n (PbO) to n (WO3) being 1 to 1, and growing the lead tungstate crystal by using a bridgman method or a czochralski method; (2) accurately orientating, cutting and grinding generated lead tungstate crystal through an X ray orientation device into lead tungstate wafers with thicknesses of 2-5mm, and cleaning the lead tungstate wafers to obtain lead tungstate crystal samples; and (3) placing the lead tungstate crystal samples obtained in the step (2) into a crucible containing metallic oxide powder to enable the lead tungstate crystal samples to be tightly wrapped by the metallic oxide powder, placing the crucible into a muffle furnace, heating the muffle furnace to 800-1000 DEG C, finishing diffusion after keeping the temperature for 12-36 hours, cooling to the room temperature, and obtaining a modified lead tungstate crystal. The process for modifying the lead tungstate crystal by utilizing the diffusion method has the advantages of low energy consumption and high efficiency.
Description
Technical field
The present invention relates to the method for the metal ion-modified crystal of lead tungstate of a kind of usefulness, belong to monocrystalline property modification technical field.
Background technology
Scintillation crystal is meant the crystal that under the irradiation of high energy particle (X ray or gamma-rays), can send UV-light or visible light; Form detector element with light-detecting device such as PM (PMT), avalanche photodiode (APD) and silicon photo diode (SPD) etc., be widely used in aspects such as high energy physics, nuclear physics, nucleus medical image and industry CT.Fast development along with the study of high energy physics project; People are for the secret of exploration of the universe space microcosm; Now building increasing large-scale accelerator of energy and hadron collider in the world, and scintillation crystal is built the important materials of the most crucial element-electromagnetic energy measuring device on these devices just.
Plumbous tungstate (being called for short PWO) crystal is as a kind of novel scintillation crystal, because its high-density (8.28g/cm
3), short radiation length (0.87cm) and Moliere radius (2.12cm), fast scintillation decay time (t
On average＜50ns), stronger radioresistance injury reinforcing ability and advantage such as cheap; Just begin the scintillation properties of systematic research PWO monocrystalline from the nineteen ninety people, be used to build the accurate electromagnetic calorimeter (ECAL) of LHC (LHC) now by CERN (CERN).Classified as one of contemporary world high-tech nine headliners' position emissron tomography (positron emission tomography by the U.S.; Be called for short PET) imaging system; Also begin to pay close attention to PWO; Japan Hamamatsu Photonics K. K has begun test the PWO crystal has been applied in the PET system, and this will cause the new upsurge of PWO scintillation crystal research.Mainly study PWO crystalline mechanism in the world Russian BTCP is arranged; France Crismatec, Ukraine Amcrys-H, German Korth and Molecular Technology; Czech Crytur; U.S. Bicron, Optocac, Shin-Etsu Chemical and domestic Shanghai silicate institute and Beijing Glass Inst. etc.The most frequently used growth method of PWO crystal has two kinds: crystal pulling method (Czochralski method) and falling crucible method (Bridgman method), mainly adopt the Czochralski grown technology, the improved Bridgman-Stockbarge method for growing technology of domestic main employing in the world.
The PWO scintillation crystal has many good qualities; But every kind of crystal and imperfect; All have the defective of self, PWO is no exception, the drawbacks limit that PWO crystal photoyield (be called for short LY) is low it in the high energy field beyond the application of other field; How to improve PWO crystalline LY to widen its Application Areas especially in the application aspect the medical imagings such as PET, this is a problem being badly in need of solution at present.At present the method for raising PWO crystal LY commonly used has: (1) is dopant ion in PWO matrix, thereby introduces new luminescence center, the first excited state radiative transition energy that makes luminescence center near or be lower than WO slightly
4 2-The zero-phonon transition energy, electronic level that dopant ion is high in addition and the strong e that catches
-Ability also can produce positive influence to the raising of PWO crystal LY; (2) through optimizing annealing process condition compensation oxygen room, reduce defective, improve near the transmitance of PWO crystal blue glow peak (420nm).But the dopant ion crystal of lead tungstate of growing; From the orientation cutting of the preparation of platinum crucible, crystal seed, charging, shove charge to crystalline intensification, inoculation, oriented growth; This all need enrich crystal of lead tungstate growth experience; And the crystal of lead tungstate of growth is difficult to obtain the high quality crystal of lead tungstate because subsurface defect and thermal stresses very easily make the generation of crystal of lead tungstate cracking and twin.
Summary of the invention
The technical problem that the present invention will solve is to provide a kind of and in crystal of lead tungstate, introduces the technology that metals ion improves the crystal of lead tungstate scintillation properties through diffusion process, has less energy-consumption, high-efficiency characteristics.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
The technology of ion diffusion modification crystal of lead tungstate may further comprise the steps:
1) with PbO powder and WO
3Powder is a raw material, according to n (PbO): n (WO
3)=1: 1 mol ratio accurate dosing utilizes falling crucible method or Czochralski grown crystal of lead tungstate;
2) with the crystal of lead tungstate that generates through the X-ray orientation device accurate pointing, cut, grind to form the plumbous tungstate wafer that thickness is 2～5mm specification, obtain pure tungsten lead plumbate crystal prototype after the cleaning;
3) the pure tungsten lead plumbate crystal prototype that step (2) is obtained is put into the crucible that metal oxide powder is housed; Make pure tungsten lead plumbate crystal prototype by the tight parcel of metal oxide powder; Then crucible is put into retort furnace, be warming up to 800～1000 ℃, diffusion finishes behind insulation 12～36h; Be cooled to room temperature then, obtain the crystal of lead tungstate of modification.The crystal of lead tungstate of the modification that makes take out after clean, optical polish can carry out the scintillation properties test.
In the said step 1), can use conventional falling crucible method or crystal pulling method to prepare crystal of lead tungstate, for example according to [Journal of Crystal Growth 2002; 236; 589-595.] and [Journal of Crystal Growth 1999,204,505-511.] disclosed method prepare.Preferred PbO powder of the present invention and WO
3The purity of powder is 99.999%.
Said step 2) in, crystal of lead tungstate is by the direction of growth (001) orientation.
In the said step 3), temperature rise rate is 12～17 ℃/min, and preferred temperature rise rate is 15 ℃/min; Cooling is for naturally cooling to room temperature.
It is analytically pure MOX: CeO that described metal oxide powder is preferably following a kind of purity
2, Cr
2O
3, Gd
2O
3, Sm
2O
3, MnO
2, Eu
2O
3
Owing to exist vacancy defect and gap in the crystal; Temperature is the main factor that influences rate of diffusion, and under the condition of high temperature, the hot activation energy of atom is big; Atoms metal gets into interstitial site, the room in the lattice easily or directly exchanges the atom in the crystal of lead tungstate; Can reduce the vacancy defect in the crystal of lead tungstate to a certain extent, form new luminescence center, thereby improve the scintillation properties of crystal of lead tungstate.Among the present invention, different metal ion diffusion temperature is different, CeO
2Diffusion temperature is preferably 1000 ℃, Cr
2O
3, Gd
2O
3, MnO
2, Eu
2O
3Diffusion temperature is preferably 900 ℃, Sm
2O
3Diffusion temperature is preferably 800 ℃.Be preferably 24-36h diffusion time.Ion diffusion is generally carried out in air atmosphere; But also can in reducing atmosphere, carry out if desired; Contain reducing gas in the said reducing atmosphere; The volume content of reducing gas≤100%, promptly described reducing atmosphere can be reducing gas or reducing gas and Air mixing, said reducing gas is CO, H for example
2, H
2S, the reducing power size in the reducing atmosphere control diffusion process of the present invention's different concns capable of using is controlled the different metal ionic valence state of introducing crystal of lead tungstate with this.
The present invention compared with prior art, its advantage is: the present invention introduces the scintillation properties that metals ion has improved crystal of lead tungstate in crystal of lead tungstate, has obtained high-quality modification crystal of lead tungstate; Equipment, technology are simple, greatly reduce energy consumption and time, have improved efficient; Can spread multiple metallic element simultaneously, and can introduce the different metal ionic valence state of crystal of lead tungstate, to improve the crystal of lead tungstate scintillation properties through reducing atmosphere control; Good reproducibility.
Description of drawings
Fig. 1 is a different metal ion diffusion modification crystal of lead tungstate equipment synoptic diagram; Crystal of lead tungstate is closely wrapped up by MOX, and a is a corundum crucible, and b is a MOX, and c is a crystal of lead tungstate.
Fig. 2 is MOX CeO among the embodiment 1
2At the modification crystal of lead tungstate of 1000 ℃ of diffusion 24h and the fluorescence spectrum of the crystal of lead tungstate that does not spread, excitation wavelength is 300nm.
Fig. 3 is MOX Cr among the embodiment 2
2O
3At the modification crystal of lead tungstate of 900 ℃ of diffusion 24h and the fluorescence spectrum of the crystal of lead tungstate that does not spread, excitation wavelength is 300nm.
Fig. 4 is MOX Sm among the embodiment 3
2O
3At the modification crystal of lead tungstate of 800 ℃ of diffusion 24h and the fluorescence spectrum of the crystal of lead tungstate that does not spread, excitation wavelength is 300nm.
Fig. 5 is MOX Eu among the embodiment 4
2O
3At the modification crystal of lead tungstate of 900 ℃ of diffusion 24h and the fluorescence spectrum of the crystal of lead tungstate that does not spread, excitation wavelength is 300nm.
Fig. 6 is embodiment 5 MOX MnO
2At the modification crystal of lead tungstate of 900 ℃ of diffusion 24h and the fluorescence spectrum of the crystal of lead tungstate that does not spread, excitation wavelength is 300nm.
Fig. 7 is MOX Gd among the embodiment 6
2O
3At the modification crystal of lead tungstate of 900 ℃ of diffusion 24h and the fluorescence spectrum of the crystal of lead tungstate that does not spread, excitation wavelength is 300nm.
Embodiment
Further set forth the present invention below in conjunction with embodiment, but should not be regarded as limitation of the scope of the invention by any way.
Embodiment 1
1, will be with the PbO powder of 99.999% purity and the WO of 99.999% purity
3Powder is a raw material, according to n (PbO): n (WO
3)=1: 1 mol ratio accurate dosing; Utilize the Bridgman-Stockbarge method for growing crystal of lead tungstate [referring to Journal of Crystal Growth 2002; 236; 589-595.], directed by the direction of growth (001), cut, grind to form the pure tungsten lead plumbate wafer of 10mm * 10mm * 2mm specification, clean and obtain pure tungsten lead plumbate crystal prototype;
2, the pure tungsten lead plumbate crystal prototype that step 1 is obtained puts into that purity is housed is analytically pure CeO
2In the corundum crucible of powder, make pure tungsten lead plumbate crystal prototype, then crucible is put into retort furnace and heat up by tight parcel (as shown in Figure 1); Temperature rise rate is 15 ℃/min, and temperature rises to 1000 ℃, insulation 24h; Cooling is for naturally cooling to room temperature, and whole diffusion atmosphere is air;
3, diffusion finishes, and crystal of lead tungstate obtains the modification crystal of lead tungstate sample that supplies performance test to use through cleaning, on polishing machine, carry out optical polish after the diffusion that step 2 is obtained, and its fluorescence spectrum figure sees Fig. 2.
Embodiment 2
1, process step is with step 1 among the embodiment 1;
2, the crystal of lead tungstate sample that step 1 is obtained puts into that purity is housed is analytical pure Cr
2O
3In the corundum crucible of powder, make the plumbous tungstate wafer by tight parcel, then crucible is put into retort furnace and heat up, temperature rise rate is 15 ℃/min, and temperature rises to 900 ℃, and insulation 24h lowers the temperature to naturally cooling to room temperature, and whole diffusion atmosphere is air;
3, process step is with step 3 among the embodiment 1.The fluorescence spectrum figure of gained modification crystal of lead tungstate sample sees Fig. 3.
1, process step is with step 1 among the embodiment 1;
2, the pure tungsten lead plumbate crystal prototype that step 1 is obtained puts into that purity is housed is analytical pure Sm
2O
3In the corundum crucible of powder, make pure tungsten lead plumbate crystal prototype by tight parcel, then crucible is put into retort furnace and heat up, temperature rise rate is 15 ℃/min, and temperature rises to 800 ℃, and insulation 24h lowers the temperature to naturally cooling to room temperature, and whole diffusion atmosphere is air;
3, process step is with step 3 among the embodiment 1.The fluorescence spectrum figure of gained modification crystal of lead tungstate sample sees Fig. 6.
Embodiment 4
1, process step is with step 1 among the embodiment 1;
2, the pure tungsten lead plumbate crystal prototype that step 1 is obtained puts into that purity is housed is analytical pure Eu
2O
3In the corundum crucible of powder, make pure tungsten lead plumbate crystal prototype, then crucible is put into retort furnace and heat up by tight parcel; Temperature rise rate is 15 ℃/min, and temperature rises to 900 ℃, insulation 24h; Cooling is for naturally cooling to room temperature, and whole diffusion atmosphere is the CO reducing atmosphere;
3, process step is with step 3 among the embodiment 1.
Embodiment 5
1, process step is with step 1 among the embodiment 1;
2, the pure tungsten lead plumbate crystal prototype that step 1 is obtained puts into that purity is housed is analytical pure MnO
2In the corundum crucible of powder, make pure tungsten lead plumbate crystal prototype by tight parcel, then crucible is put into retort furnace and heat up, temperature rise rate is 15 ℃/min, and temperature rises to 900 ℃, and insulation 24h lowers the temperature to naturally cooling to room temperature, and whole diffusion atmosphere is air;
3, process step is with step 3 among the embodiment 1.
Embodiment 6
1, process step is with step 1 among the embodiment 1;
2, the pure tungsten lead plumbate crystal prototype that step 1 is obtained puts into that purity is housed is analytical pure Gd
2O
3In the corundum crucible of powder, make pure tungsten lead plumbate crystal prototype by tight parcel, then crucible is put into retort furnace and heat up, temperature rise rate is 15 ℃/min, and temperature rises to 900 ℃, and insulation 24h lowers the temperature to naturally cooling to room temperature, and whole diffusion atmosphere is air;
3, process step is with step 3 among the embodiment 1.
Claims (10)
1. the technology of ion diffusion modification crystal of lead tungstate may further comprise the steps:
1) with PbO powder and WO
3Powder is a raw material, according to n (PbO): n (WO
3)=1: 1 mol ratio accurate dosing utilizes falling crucible method or Czochralski grown crystal of lead tungstate;
2) with the crystal of lead tungstate that generates through the X-ray orientation device accurate pointing, cut, grind to form the plumbous tungstate wafer that thickness is 2～5mm specification, obtain pure tungsten lead plumbate crystal prototype after the cleaning;
3) the pure tungsten lead plumbate crystal prototype that step (2) is obtained is put into the crucible that metal oxide powder is housed; Make pure tungsten lead plumbate crystal prototype by the tight parcel of metal oxide powder; Then crucible is put into retort furnace, be warming up to 800～1000 ℃, diffusion finishes behind insulation 12～36h; Be cooled to room temperature then, obtain the crystal of lead tungstate of modification.
2. the technology of ion diffusion modification crystal of lead tungstate as claimed in claim 1 is characterized in that: in the said step 3), temperature rise rate is 12～17 ℃/min; Cooling is for naturally cooling to room temperature.
3. the technology of ion diffusion modification crystal of lead tungstate as claimed in claim 2 is characterized in that: temperature rise rate is 15 ℃/min.
4. like the technology of the described ion diffusion modification of one of claim 1～3 crystal of lead tungstate, it is characterized in that: it is analytically pure MOX: CeO that described metal oxide powder is selected from following a kind of purity
2, Cr
2O
3, Gd
2O
3, Sm
2O
3, MnO
2, Eu
2O
3
5. the technology of ion diffusion modification crystal of lead tungstate as claimed in claim 4 is characterized in that: described metal oxide powder is analytically pure CeO
2, diffusion temperature is 1000 ℃.
6. the technology of ion diffusion modification crystal of lead tungstate as claimed in claim 4 is characterized in that: it is analytically pure MOX: Cr that described metal oxide powder is selected from following a kind of purity
2O
3, Gd
2O
3, MnO
2, Eu
2O
3, diffusion temperature is 900 ℃.
7. the technology of ion diffusion modification crystal of lead tungstate as claimed in claim 4 is characterized in that: described metal oxide powder is analytically pure Sm
2O
3, diffusion temperature is 800 ℃.
8. like the technology of the described ion diffusion modification of one of claim 5～7 crystal of lead tungstate, it is characterized in that: be 24-36h diffusion time.
9. like the technology of the described ion diffusion modification of one of claim 1～3 crystal of lead tungstate, it is characterized in that: in the said step 3), be diffused in the air atmosphere or carry out in the reducing atmosphere.
10. the technology of ion diffusion modification crystal of lead tungstate as claimed in claim 9 is characterized in that: described reducing atmosphere contains reducing gas, and said reducing gas is CO, H
2Or H
2S, the volume content of reducing gas≤100% in the said reducing atmosphere.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102774888A (en) * | 2012-07-31 | 2012-11-14 | 中国科学院化学研究所 | Method for preparing lead tungstate nano-powder |
| CN110607560A (en) * | 2019-09-29 | 2019-12-24 | 宁波阳光和谱光电科技有限公司 | Oxygen supplementing and color reducing growth method of cadmium tungstate scintillation single crystal |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102774888A (en) * | 2012-07-31 | 2012-11-14 | 中国科学院化学研究所 | Method for preparing lead tungstate nano-powder |
| CN102774888B (en) * | 2012-07-31 | 2014-08-27 | 中国科学院化学研究所 | Method for preparing lead tungstate nano-powder |
| CN110607560A (en) * | 2019-09-29 | 2019-12-24 | 宁波阳光和谱光电科技有限公司 | Oxygen supplementing and color reducing growth method of cadmium tungstate scintillation single crystal |
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