CN101235545A - Cesium tungstate scintillation crystal and its preparation method and application - Google Patents
Cesium tungstate scintillation crystal and its preparation method and application Download PDFInfo
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- CN101235545A CN101235545A CNA2007101565589A CN200710156558A CN101235545A CN 101235545 A CN101235545 A CN 101235545A CN A2007101565589 A CNA2007101565589 A CN A2007101565589A CN 200710156558 A CN200710156558 A CN 200710156558A CN 101235545 A CN101235545 A CN 101235545A
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Abstract
The invention discloses tungstic acid cesium flickering crystal and a papering method and application thereof for the tungstic acid cesium flickering crystal, wherein the chemical composition of the crystal is Cs2W2O7, the poly-crystal of the composition is prepared by the solid-phase sintering method and the single-crystal of the composition is prepared by the bridgman method, wherein the physicochemical property of the tungstic acid cesium Cs2W2O7 crystal is steady, the tungstic acid cesium Cs2W2O7 crystal dose not need any surface protection when being used, the material of the Cs2W2O7 is intrinsic luminescence scintillator material, and the luminescence group of the Cs2W2O7 is a W2O72-group, no need of any doping ion, the energy resolution capability of the tungstic acid cesium flickering crystal can not be interfered, and the tungstic acid cesium flickering crystal emits a strong light under stimulating by the X-ray, and the luminescence wavelength of the crystal can be coupled well with the existing electron-multiplier phototube, furthermore, the row material of the Cs2W2O7 is relative cheaper, in the foreseeable future, the single-crystal and the poly-crystal of the Cs2W2O7 can be extensively applied in the X-ray, the gamma-ray and nuclear radiation probing field and the like.
Description
Technical field
The present invention relates to scintillator crystal materials, especially relate to a kind of cesium tungstate scintillation crystal and preparation method thereof and application.
Background technology
High energy ray or particles such as scintillation crystal can detecting x-ray, gamma-rays, alpha-particle, at medical diagnosis (X-CT, PET, SPECT etc.), safety inspection (inspection of containers, row bag check etc.), oil well exploration (oil well the is surveyed probe) field of waiting have obtained in a large number application widely.Present commercial scintillation crystal is a lot, but almost each all has apparent in view shortcoming, so its Application Areas is all relatively limited.NaI:Tl (sodium iodide,crystal) crystal of being found by RobertHofstadter in 1948 is the big breakthrough in scintillation crystal field, and this crystal has very high light output, is still used in a large number up to now.But this crystallo-luminescence decay is slow, and anti-irradiation ability is poor, be very easy to deliquescence, and doping agent Tl (thallium) toxicity that this crystal is rely luminous is very big.The discovery of NaI:Tl scintillation crystal has promoted the development of alkali halogen compound series scintillation crystal, as CsI:Tl (cesium iodide,crystal) crystal, CsI:Na (mixing the sodium cesium iodide) crystal or the like.These alkali halogen compound serial crystals have and the similar relative merits of NaI:Tl scintillation crystal.The Lu that find the nineties in last century
2SiO
5: Ce (mixing cerium silicic acid lutetium) crystal is the another important invention in scintillation crystal field, this crystalline decay of luminescence is fast, anti-irradiation ability is strong, but this crystal is a raw material with the precious metal lutetium, and fusing point height (＞2000 ℃) causes that to produce power consumption big, so price is very expensive, and the skewness of light emitting ionic in matrix can reduce its energy resolution ability, Lu has radio isotope in addition, can produce noise signal, also is a shortcoming.The LaCl that find the beginning of this century
3: Ce (Ce-doped lanthanum oxide) and LaBr
3: Ce (mixing the cerium lanthanum bromide) crystal is the most important discovery in scintillation crystal field recent years, and this two kinds of crystalline light output is all very high, and decay of luminescence is very fast, but as easy as rolling off a log generation deliquescence and problem of oxidation, and the cost that is used for making detector is very high.
Summary of the invention
The object of the present invention is to provide a kind of wolframic acid caesium (Cs
2W
2O
7) scintillation crystal and preparation method thereof and application.
The technical solution used in the present invention is:
One, a kind of cesium tungstate scintillation crystal material:
Its chemical composition is Cs
2W
2O
7Described Cs
2W
2O
7Material is monocrystalline or polycrystalline.
Two, a kind of Cs
2W
2O
7The preparation method of polycrystalline material, the step of this method is as follows:
Purity is the WO more than 99.9%
3And Cs
2CO
3Be raw material, according to material mol ratio WO
3: Cs
2CO
3Mix be placed in platinum crucible at=2: 1, platinum crucible is put in the muffle furnace in 750～950 ℃ to react 8～12 hours again, obtains Cs
2W
2O
7The polycrystal material piece;
Three, a kind of Cs
2W
2O
7The preparation method of monocrystal material, the step of this method is as follows:
1 seed crystal for preparing is in advance put into the bottom of platinum crucible, again with Cs
2W
2O
7Polycrystal material is packaged to be entered in the platinum crucible, then platinum crucible is packaged the crucible tight seal;
2 corundum that above-mentioned platinum crucible is fixed in the crystal decline stove draw on the lower pipe, and its position is the high-temperature region at the upper area of crystal decline stove, and corundum draws lower pipe and draws lower mechanism and link to each other;
3 are raised to 800～1000 ℃ with the descend temperature of stove of crystal, are incubated 10～14 hours, make the Cs in the platinum crucible
2W
2O
7The material piece all melts simultaneously, and the part seed crystal also melts;
4 slow decreasings draw lower pipe, and decrease speed is 1～2mm/h, and this moment, solid liquid interface was positioned at the temperature gradient zone of stove, and thermograde is 30 ℃～40 ℃/cm, and along with the continuous decline of crucible, crystallization goes out Cs gradually
2W
2O
7Monocrystalline;
After 5 crystal growths are finished, furnace temperature is reduced to normal temperature gradually with 8～15 ℃/hour speed.
Four, a kind of application of cesium tungstate scintillation crystal material:
The application of cesium tungstate scintillation crystal material in nuclear radiation detector.Described nuclear radiation detector be applied as application in X ray or the gamma detector.
The present invention compares with background technology, and the beneficial effect that has is:
Wolframic acid caesium Cs
2W
2O
7The crystal physical and chemical performance is stable, need not any surface protection during use, and Cs
2W
2O
7Be the luminous scintillator material of intrinsic, its luminophore is W
2O
7 2-Group need not any doping ion, and the energy resolution ability is not disturbed by this can, and its luminous very strong under excitation of X-rays, emission wavelength can with the well coupling of existing photomultiplier.In addition, consist of Cs
2W
2O
7Raw material all relatively cheap.Can predict Cs
2W
2O
7Monocrystalline or polycrystalline will be widely used in nuclear radiation detection fields such as X, gamma-rays.
Description of drawings
Accompanying drawing is wolframic acid caesium (Cs of the present invention
2W
2O
7) the gamma-rays exciting light output test spectral of crystal.
Embodiment
The invention will be further described below in conjunction with drawings and Examples.
Embodiment 1:
Wolframic acid caesium (Cs
2W
2O
7) solid phase of polycrystalline is synthetic.
Take by weighing purity and be higher than 99.9% Tungsten oxide 99.999 (WO
3) 10 grams, purity is higher than 99.9% cesium carbonate 7.0266 grams, and fully ground and mixed is placed in the platinum crucible, platinum crucible is placed muffle furnace to rise to 900 ℃ of high temperature sinterings, synthesised polycrystalline again.
Embodiment 2:
Wolframic acid caesium (Cs
2W
2O
7) solid phase of polycrystalline is synthetic.
Take by weighing purity and be higher than 99.9% Tungsten oxide 99.999 (WO
3) 30 grams, purity is higher than 99.9% cesium carbonate 21.0798 grams, and fully ground and mixed is placed in the platinum crucible, places muffle furnace to rise to 900 ℃ of high temperature sinterings, synthesised polycrystalline platinum crucible.
Embodiment 3:
Wolframic acid caesium (Cs
2W
2O
7) crucible lowering method crystal growth of monocrystalline.
1. make the capillary platinum crucible, this capillary platinum crucible is characterised in that its afterbody part internal diameter has only 53mm, and length is 5cm, and the internal diameter of its main part is 3cm, and length is 20cm.
2. pack into after the polycrystalline powder among the embodiment 1 fully being ground in the above-mentioned platinum crucible, platinum crucible is tightly encapsulated.
3. with 60 ℃ heat-up rate per hour growth furnace is raised to 900 ℃, is incubated 12 hours.Pipe is until finishing crystal growth under drawing with 1.0mm/ hour the slow decline of speed then, and the thermograde of growth interface is controlled at～30 ℃/cm.
4. after crystal growth is finished, furnace temperature is reduced to 700 ℃ respectively with 10 ℃/hour speed, 500 ℃, 300 ℃, and, with 10 ℃/hour temperature control the crystal furnace temperature is reduced to room temperature then said temperature constant temperature 8 hours, take out crystal.
5. the present embodiment growth obtains being of a size of the Cs of 20 * 25mm
2W
2O
7Transparent crystal.
Embodiment 4:
Wolframic acid caesium (Cs
2W
2O
7) crucible lowering method crystal growth of monocrystalline.
1. be the crucible that the platinized platinum of 0.1mm is made 20 * 20 * 200mm with thickness, and with the Cs that obtains among the embodiment 3
2W
2O
7Transparent crystal is processed into the Cs that is of a size of 20 * 15mm
2W
2O
7Monocrystalline is placed on the bottom of crucible, and suitably the mycrodyne crucible bottom makes seed crystal and crucible close contact then, packs into after the polycrystalline powder among the embodiment 2 fully being ground in the above-mentioned platinum crucible again, and platinum crucible is tightly encapsulated.
2. 3,4 among crystal growing process such as the embodiment 3.
3. the growth of this example obtains transparent Cs
2W
2O
7Crystal, size reach 20 * 80mm.The crystal photoyield reaches 200P.e/MeV.Crystalline gamma-rays excitation spectrum as shown in Figure 1.
Embodiment 5:
Cs
2W
2O
7The application of monocrystalline in X-ray detector
With the Cs that obtains among the embodiment 4
2W
2O
7Crystal is processed into the quartz crystal device of 3 * 3 * 20mm, and 128 these quartz crystal devices are made a Flat X-ray detector, and the X ray energy linearity resolution capability of detector is good.
Claims (6)
1, a kind of cesium tungstate scintillation crystal material is characterized in that: its chemical composition is Cs
2W
2O
7
2, a kind of cesium tungstate scintillation crystal material according to claim 1 is characterized in that: described Cs
2W
2O
7Material is monocrystalline or polycrystalline.
3, a kind of wolframic acid caesium polycrystalline preparation method is characterized in that the step of this method is as follows:
Purity is the WO more than 99.9%
3And Cs
2CO
3Be raw material, according to material mol ratio WO
3: Cs
2CO
3Mix be placed in platinum crucible at=2: 1, places muffle furnace to react 8～12 hours in 750～950 ℃ again, obtains Cs
2W
2O
7The polycrystal material piece.
4, a kind of preparation method of wolframic acid caesium monocrystalline is characterized in that:
1) seed crystal for preparing is in advance put into the bottom of platinum crucible, again with Cs
2W
2O
7Polycrystal material is packaged to be entered in the platinum crucible, then platinum crucible is packaged the crucible tight seal;
2) corundum that above-mentioned platinum crucible is fixed in the crystal decline stove draws on the lower pipe, and its position is the high-temperature region at the upper area of crystal decline stove, and corundum draws lower pipe and draws lower mechanism and link to each other;
3) crystal the is descended temperature of stove is raised to 800～1000 ℃, is incubated 10～14 hours, makes the Cs in the platinum crucible
2W
2O
7The material piece all melts simultaneously, and the part seed crystal also melts;
4) slow decreasing draws lower pipe, and decrease speed is 1～2mm/h, and this moment, solid liquid interface was positioned at the temperature gradient zone of crystal decline stove, and thermograde is 30 ℃～40 ℃/cm, and along with the continuous decline of crucible, crystallization goes out Cs gradually
2W
2O
7Monocrystalline;
5) after crystal growth is finished, the descend furnace temperature of stove of crystal is reduced to normal temperature gradually with 8～15 ℃/hour speed.
5, a kind of application of cesium tungstate scintillation crystal material is characterized in that: the application of cesium tungstate scintillation crystal material in nuclear radiation detector.
6, the application of a kind of cesium tungstate scintillation crystal material according to claim 5 is characterized in that: described nuclear radiation detector be applied as application in X ray or the gamma detector.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101565589A CN101235545A (en) | 2007-11-08 | 2007-11-08 | Cesium tungstate scintillation crystal and its preparation method and application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101565589A CN101235545A (en) | 2007-11-08 | 2007-11-08 | Cesium tungstate scintillation crystal and its preparation method and application |
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|---|---|
| CN101235545A true CN101235545A (en) | 2008-08-06 |
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105664920A (en) * | 2016-01-30 | 2016-06-15 | 苏州大学 | Cs2W3O10 (cesium tungstate) powder, preparation method and application thereof |
| WO2023060337A1 (en) * | 2021-10-11 | 2023-04-20 | Electrochem Technologies & Materials Inc. | High temperature chemical process for the preparation of cesium tungstate |
-
2007
- 2007-11-08 CN CNA2007101565589A patent/CN101235545A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105664920A (en) * | 2016-01-30 | 2016-06-15 | 苏州大学 | Cs2W3O10 (cesium tungstate) powder, preparation method and application thereof |
| WO2023060337A1 (en) * | 2021-10-11 | 2023-04-20 | Electrochem Technologies & Materials Inc. | High temperature chemical process for the preparation of cesium tungstate |
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Open date: 20080806 |