CN104357903A - Calcium fluoride crystal containing europium, preparation method and application - Google Patents
Calcium fluoride crystal containing europium, preparation method and application Download PDFInfo
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- CN104357903A CN104357903A CN201410575257.XA CN201410575257A CN104357903A CN 104357903 A CN104357903 A CN 104357903A CN 201410575257 A CN201410575257 A CN 201410575257A CN 104357903 A CN104357903 A CN 104357903A
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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
- C30B29/12—Halides
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/16—Measuring radiation intensity
- G01T1/20—Measuring radiation intensity with scintillation detectors
- G01T1/202—Measuring radiation intensity with scintillation detectors the detector being a crystal
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Abstract
The invention relates to the technical field of crystal growth, in particular to a calcium fluoride crystal containing europium, a preparation method and application. The calcium fluoride crystal containing europium, provided by the invention, can be irradiate with Co60; the light yield of the crystal is measured with an RCA8850 photomultiplier; the result shows that the calcium fluoride crystal containing europium, provided by the invention, has the excellent scintillating crystal property of emitting twinkling fluorescent light of a certain wave length after absorbing the energy of high-energy particles on the condition that the content of the crystal is low. Especially, the relative light output of the crystal is equal to that of an LYSO scintillating crystal. Besides, as the content is low, the calcium fluoride crystal containing europium is beneficial to growth of high optical mass crystals. The invention further provides the preparation method and the application of the calcium fluoride crystal containing europium.
Description
Technical field
The present invention relates to technical field of crystal growth, be specifically related to a kind of calcium fluoride crystal, Preparation method and use containing europium.
Background technology
In prior art, scintillation crystal sends the crystal of certain wavelength blinking after can absorbing high energy particle energy, through photo-translating system and auxiliary electronic equipment, finally can determine the energy of high energy particle.Scintillation crystal can be used for the detection of X-ray, gamma-rays, neutron and other high energy particles.Calcium fluoride crystal is a kind of multi-functional, multiduty crystalline material, there is its own mechanical stable performance, easily processing, not deliquescence, low in raw material price, easily growing large-size monocrystalline a little, be one of current most widely used optical crystal, but pure calcium fluoride crystal does not have the performance sending certain wavelength blinking after scintillation crystal absorbs high energy particle energy.
Summary of the invention
In order to overcome defect of the prior art, the invention provides a kind of calcium fluoride crystal, Preparation method and use containing europium, solving pure calcium fluoride crystal and not there is the problem sending certain wavelength blinking performance after scintillation crystal absorbs high energy particle energy.
The present invention is achieved through the following technical solutions: a kind of calcium fluoride crystal containing europium, comprise calcium fluoride crystal, described crystal comprises europium element.
Further, described europium element adds in described calcium fluoride crystal in the mode of europium.
Further, in described calcium fluoride crystal, europium content range mass percent is 0.5 × 10
-3wt% ~ 5 × 10
-3wt%.
Further, in described calcium fluoride crystal, europium content range mass percent is 0.5 × 10
-3wt% ~ 2 × 10
-3wt%.
Further, in described calcium fluoride crystal, europium content mass percent is 0.5 × 10
-3wt%, 1 × 10
-3wt% or 2 × 10
-3wt%.
Further, a kind of calcium fluoride crystal preparation method containing europium, said method comprising the steps of:
Step one, the Calcium Fluoride (Fluorspan) getting arbitrary described content range and europium powder fully mix, and obtain mixture, be loaded in vacuum drying oven, dry 12 hours, obtain combinations raw material under 200 DEG C of conditions after described mixture is left standstill 24 hours;
Step 2, the described combinations raw material described step one obtained load plumbago crucible, and are positioned in crystal growing furnace by crucible, and in described crystal growing furnace stove, vacuum is evacuated to 1.0 × 10
-3pa, is warming up to melting sources, is declined by described plumbago crucible with the speed of 5mm/h, is down to room temperature and obtains crystallization raw material after described combinations raw material is completely by gradient zones;
Step 3, take out described crystallization raw material, remove the part that described crystallization raw material top impurity is more, obtain the Calcium Fluoride (Fluorspan) polycrystal raw material containing europium, obtain polycrystal raw material powder after being pulverized by described polycrystal raw material and be used for crystal growth;
Step 4, by described polycrystal raw material powder, crystal pulling method or falling crucible method is adopted to be prepared into the described calcium fluoride crystal containing europium.
Further, described falling crucible method comprises the following steps:
Step one, the plumbous fluoride that described polycrystal raw material powder adds 1 ~ 2wt% is mixed after put into plumbago crucible, described plumbago crucible is put into decline stove, and crystal growth direction is <100> or <111>;
Step 2, vacuumize and make furnace interior vacuum tightness reach 1.0 × 10
-3more than Pa;
Step 3, plumbago crucible lowering speed are 1 ~ 2mm/h;
Step 4, temperature gradient of solid-liquid interface are 20 DEG C/cm;
Be cooled to room temperature with the speed of 30 DEG C/h after step 5, crystal growth terminate, obtain the calcium fluoride crystal raw material containing europium;
Step 6, described crystal raw material carried out successively anneal, directed, cutting, grinding and polished finish, obtain content for (mass percent) 0.5 × 10
-3wt% ~ 5 × 10
-3the calcium fluoride crystal containing europium of wt%.
Further, described crystal pulling method comprises the following steps:
Step one, the plumbous fluoride that described polycrystal raw material powder adds 1 ~ 2wt% is mixed after put into loading plumbago crucible, described plumbago crucible is put into decline stove, and crystal growth direction is <100> or <111>;
Step 2, vacuumize and make furnace interior vacuum tightness reach 3.0 × 10
-3more than Pa, after be filled with argon gas and tetrafluoro-methane mixed gas as protective atmosphere;
Step 3, make crystal pull rate be 2 ~ 3mm/h, speed of rotation 20 ~ 30r/min, temperature gradient of solid-liquid interface is 10 DEG C/cm;
Room temperature is cooled to the speed of 30 DEG C/h after step 4, crystal growth terminate;
Step 5, above-mentioned crystal is annealed successively, directed, cutting, grinding and polished finish, obtain content for (mass percent) 0.5 × 10
-3wt% ~ 5 × 10
-3the calcium fluoride crystal containing europium of wt%.
Further, a kind of calcium fluoride crystal purposes containing europium, the described calcium fluoride crystal containing europium is made into scintillation crystal.
Further, described scintillation crystal is made into scintillation crystal detectors.
Compared with prior art, superior effect is: the calcium fluoride crystal containing europium provided by the invention can use Co60 to irradiate, by the photoyield of RCA8850 photomultiplier measurement crystal, result shows that the calcium fluoride crystal containing europium provided by the invention is 0.5 × 10 at content
-3wt% ~ 5 × 10
-3when wt%, it is suitable that calcium fluoride crystal is provided with the relative root mean square error that sends the performance, particularly crystal of certain wavelength blinking after excellent scintillation crystal absorbs high energy particle energy and yttrium luetcium silicate (LYSO) crystal that glimmers.In addition, because content is low, it is also beneficial to the crystal of growth high optical quality.
Accompanying drawing explanation
Fig. 1 is the calcium fluoride crystal radioluminescence spectrogram containing europium of the present invention.
Reference numeral is as follows
Fig. 1 transverse axis is the wavelength/nanometer value (Vavelength/nm) of the calcium fluoride crystal containing europium of the present invention;
Fig. 1 longitudinal axis is the intensity/relative unit value (Intensity/au) of the calcium fluoride crystal ray containing europium of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the invention is described in further detail.
The invention provides a kind of calcium fluoride crystal containing europium, comprise calcium fluoride crystal, described crystal comprises europium element, and described europium element adds in described calcium fluoride crystal in the mode of europium, and in described calcium fluoride crystal, europium content range (mass percent) is 0.5 × 10
-3wt% ~ 5 × 10
-3wt%, in described calcium fluoride crystal, europium content range (mass percent) is 0.5 × 10
-3wt% ~ 2 × 10
-3wt%, europium content (mass percent) preferably 0.5 × 10 in described calcium fluoride crystal
-3wt%, 1 × 10
-3wt% or 2 × 10
-3wt%.
Present invention also offers a kind of calcium fluoride crystal preparation method containing europium, said method comprising the steps of:
Step one, the Calcium Fluoride (Fluorspan) getting described arbitrary content range and europium powder fully mix, and obtain mixture, be loaded in vacuum drying oven, dry 12 hours, obtain combinations raw material under 200 DEG C of conditions after described mixture is left standstill 24 hours;
Step 2, the described combinations raw material described step one obtained load plumbago crucible, and are positioned in crystal growing furnace by described crucible, and in described crystal growing furnace stove, vacuum is evacuated to 1.0 × 10
-3pa, is warming up to melting sources, and crucible declines with the speed of 5mm/h, is down to room temperature and obtains crystallization raw material after described combinations raw material is completely by gradient zones;
Step 3, take out described crystallization raw material, remove the part that described crystallization raw material top impurity is more, obtain the Calcium Fluoride (Fluorspan) polycrystal raw material containing europium, obtain polycrystal raw material powder after being pulverized by described polycrystal raw material and be used for crystal growth;
Step 4, by described polycrystal raw material powder, crystal pulling method or falling crucible method is adopted to be prepared into the described calcium fluoride crystal containing europium.
Described falling crucible method comprises the following steps:
Step one, the plumbous fluoride that described polycrystal raw material powder adds 1 ~ 2wt% is mixed after put into plumbago crucible, described plumbago crucible is put into decline stove, and crystal growth direction is <100> or <111>;
Step 2, vacuumize and make furnace interior vacuum tightness reach 1.0 × 10
-3more than Pa;
Step 3, described plumbago crucible lowering speed are 1 ~ 2mm/h;
Step 4, temperature gradient of solid-liquid interface are 20 DEG C/cm;
Be cooled to room temperature with the speed of 30 DEG C/h after step 5, crystal growth terminate, obtain the calcium fluoride crystal raw material containing europium;
Step 6, described crystal raw material carried out successively anneal, directed, cutting, grinding and polished finish, obtain content for (mass percent) 0.5 × 10
-3wt% ~ 5 × 10
-3the calcium fluoride crystal containing europium of wt%.
Described crystal pulling method comprises the following steps:
Step one, the plumbous fluoride that described polycrystal raw material powder adds 1 ~ 2wt% is mixed after put into plumbago crucible, described plumbago crucible is put into decline stove, and crystal growth direction is <100> or <111>;
Step 2, vacuumize and make furnace interior vacuum tightness reach 3.0 × 10
-3more than Pa, after be filled with argon gas and tetrafluoro-methane mixed gas as protective atmosphere;
Step 3, make crystal pull rate be 2 ~ 3mm/h, speed of rotation 20 ~ 30r/min, temperature gradient of solid-liquid interface is 10 DEG C/cm;
Room temperature is cooled to the speed of 30 DEG C/h after step 4, crystal growth terminate;
Step 5, above-mentioned crystal is annealed successively, directed, cutting, grinding and polished finish, obtain content for (mass percent) 0.5 × 10
-3wt% ~ 5 × 10
-3the calcium fluoride crystal containing europium of wt%.
Present invention also offers a kind of calcium fluoride crystal purposes containing europium, the described calcium fluoride crystal containing europium is made into scintillation crystal, and described scintillation crystal is made into scintillation crystal detectors.
Embodiment 1
A kind of calcium fluoride crystal preparation method containing europium provided by the invention, specifically according to following steps, described preparation method comprises:
Step one, get 1 kilogram of europium content (mass percent) 0.5 × 10
-3be loaded in vacuum drying oven after the Calcium Fluoride (Fluorspan) of wt% and europium powder fully mix 24 hours, dry 12 hours under 200 DEG C of conditions;
Step 2, in calcium fluoride crystal, europium content is 0.5g, and other are calcium fluoride crystal;
Step 3, employing crucible decline <Bridgman-Stockbarge> legal system are standby.
Falling crucible method <Bridgman-Stockbarge> comprises the following steps:
1) plumbous fluoride that the polycrystal raw material of 1 kilogram that above-mentioned steps is obtained adds 1 gram mixes puts into plumbago crucible, described plumbago crucible is put into decline stove, and crystal growth direction is <100> or <111>;
2) vacuumize and make furnace interior vacuum tightness reach 1 × 10
-3pa;
3) dropping speed of the crucible is 1mm/h;
4) temperature gradient of solid-liquid interface is 20 DEG C/cm;
5) crystal growth is cooled to room temperature with the speed of 30 DEG C/h after terminating;
6) crystal obtained above-mentioned steps is annealed successively, directed, cutting, grinding and polished finish, obtaining doping is (mass percent) 0.5 × 10
-3the calcium fluoride crystal containing europium of wt%.Crystal orientation: first adopt the method for measuring of " ten " word to determine the <100> crystal face or <111> crystal face of mixing europium calcium fluoride crystal with X-ray orientation device, and mark at plane of crystal;
Crystal-cut: be first <100> or crystal face along the crystal face of mark with inner circle cutting machine according to zinc germanium phosphide optical parametric oscillation element dimensional requirement be that crystal ingot is cut into wafer by <111>;
Crystal grinds: the logical light face polishing machine of crystal blank step 2 cut out, temperature be 25 DEG C ~ 28 DEG C, grinding pressure is 100g/cm
2~ 200g/cm
2, rotating speed is under the condition of 40 ~ 50 revs/min, use W10 and W3.5 abrasive lapping successively, milling time is 20min ~ 50min, makes logical light face any surface finish, without obvious cut;
Polishing crystal: temperature be 25 DEG C ~ 28 DEG C, polish pressure is 100g/cm
2~ 500g/cm
2, rotating speed is under the condition of 40 ~ 50 revs/min, taking glycerine as refrigerant, with pitch dish for polishing disk, is the polishing fluid polishing of 1 μm and 0.5 μm by abrasive grain by the logical light face polishing machine of the crystal blank through step 3 rough polishing successively.
Embodiment 2
Present invention also offers a kind of calcium fluoride crystal preparation method containing europium, described preparation method comprises:
Step one, feed pretreatment step: Calcium Fluoride (Fluorspan) and the europium powder of getting 1 kilogram, content is (mass percent) 5 × 10
-3wt%, fully mixing was loaded in vacuum drying oven after 24 hours, and dry 12 hours under 200 DEG C of conditions, wherein in calcium fluoride crystal, europium content is 5g, and all the other 995 grams is calcium fluoride crystal;
Step 2,1 kilogram of combinations raw material step one obtained load plumbago crucible, and are positioned in crystal growing furnace by described plumbago crucible, and in described crystal growing furnace stove, vacuum is evacuated to 2 × 10
-3pa, is warming up to melting sources, and plumbago crucible declines with the speed of 5mm/h, is down to room temperature and obtains crystallization raw material after described combinations raw material is completely by gradient zones;
Step 3, take out described crystallization raw material, remove the part that described crystallization raw material top impurity is more, obtain the Calcium Fluoride (Fluorspan) polycrystal raw material containing europium, obtain polycrystal raw material powder after being pulverized by described polycrystal raw material and be used for crystal growth;
Step 4, by described polycrystal raw material powder, crystal pulling method is adopted to be prepared into the described calcium fluoride crystal containing europium.
Lift <Czochralski> method in the preparation method containing europium calcium fluoride crystal provided by the invention comprises the following steps:
1) plumbago crucible is put into after plumbous fluoride polycrystal raw material being added 2 grams mixes, described plumbago crucible is put into decline stove, and crystal growth direction is <100> or <111>;
2) vacuumize and make furnace interior vacuum tightness reach 3 × 10
-3after more than Pa, be filled with argon gas and tetrafluoro-methane mixed gas as protective atmosphere;
3) crystal pull rate is 3mm/h, speed of rotation 30r/min, and temperature gradient of solid-liquid interface is 10 DEG C/cm;
4) crystal growth is cooled to room temperature with the speed of 30 DEG C/h after terminating;
5> anneals successively to above-mentioned crystal, directed, cutting, grinding and polished finish, obtain europium content for (mass percent) 5 × 10
-3the calcium fluoride crystal containing europium of wt%.
Embodiment 3
Present invention also offers a kind of calcium fluoride crystal preparation method prepared containing europium, described preparation method comprises:
1) feed pretreatment step: Calcium Fluoride (Fluorspan) and the europium powder of getting 1kg, europium content is (mass percent) 1.0 × 10
-3wt%, fully mixing was loaded in vacuum drying oven after 24 hours, dried 12 hours under 200 DEG C of conditions;
2) in said mixture calcium fluoride crystal, europium is 1 gram, and other are 999 grams;
3> adopts crystal pulling method to be prepared.
Crystal pulling method in the preparation method containing europium calcium fluoride crystal provided by the invention comprises the following steps:
1) 1kg polycrystal raw material above-mentioned steps obtained adds after plumbous fluoride 2 grams mixes puts into plumbago crucible, and be put into by described plumbago crucible in decline stove, crystal growth direction is <100>;
2) vacuumize and make furnace interior vacuum tightness reach 5 × 10
-3after Pa, be filled with argon gas and tetrafluoro-methane mixed gas as protective atmosphere;
3) crystal pull rate is 1.5mm/h, speed of rotation 25r/min, and temperature gradient of solid-liquid interface is 10 DEG C/cm;
4) crystal growth is cooled to room temperature with the speed of 30 DEG C/h after terminating;
5) crystal obtained above-mentioned steps is annealed successively, directed, cutting, grinding and polished finish, obtaining content amount is 1.0 × 10
-3the calcium fluoride crystal containing europium of wt%.
The calcium fluoride crystal purposes containing europium that the present invention makes, the described calcium fluoride crystal containing europium is made into scintillation crystal, and described scintillation crystal is made into scintillation crystal detectors.As shown in Figure 1, described scintillation crystal is used for the detection of charged ion in low-energyγ-ray, charged particle detection, dark matter detection, nuclear reactor, the monitoring of environmental radiation or radioactive medical diagnostics.
The present invention is not limited to above-mentioned embodiment, and when not deviating from flesh and blood of the present invention, any distortion that it may occur to persons skilled in the art that, improvement, replacement all fall into scope of the present invention.
Claims (10)
1., containing a calcium fluoride crystal for europium, comprise calcium fluoride crystal, it is characterized in that, described crystal comprises europium element.
2., according to claim 1 containing the calcium fluoride crystal of europium, it is characterized in that, described europium element adds in described calcium fluoride crystal in the mode of europium.
3., according to claim 2 containing the calcium fluoride crystal of europium, it is characterized in that, in described calcium fluoride crystal, europium content range mass percent is 0.5 × 10
-3wt% ~ 5 × 10
-3wt%.
4., according to claim 3 containing the calcium fluoride crystal of europium, it is characterized in that, in described calcium fluoride crystal, europium content range mass percent is 0.5 × 10
-3wt% ~ 2 × 10
-3wt%.
5., according to claim 4 containing the calcium fluoride crystal of europium, it is characterized in that, in described calcium fluoride crystal, europium content mass percent is 0.5 × 10
-3wt%, 1 × 10
-3wt% or 2 × 10
-3wt%.
6., containing a calcium fluoride crystal preparation method for europium, it is characterized in that, said method comprising the steps of:
Step one, the Calcium Fluoride (Fluorspan) getting the arbitrary described content range of claim 3 to 5 and europium powder fully mix, and obtain mixture, be loaded in vacuum drying oven, dry 12 hours, obtain combinations raw material under 200 DEG C of conditions after described mixture is left standstill 24 hours;
Step 2, the combinations raw material described step one obtained load plumbago crucible, and are positioned in crystal growing furnace by described plumbago crucible, and in described crystal growing furnace stove, vacuum tightness is evacuated to 1.0 × 10
-3more than P, post-heating is warming up to raw material and all melts, and described plumbago crucible declines with the speed of 5mm/h, is down to room temperature and obtains crystallization raw material after described combinations raw material is completely by gradient zones;
Step 3, take out described crystallization raw material, remove the part that described crystallization raw material top impurity is more, obtain the Calcium Fluoride (Fluorspan) polycrystal raw material containing europium, obtain polycrystal raw material powder after being pulverized by described polycrystal raw material and be used for crystal growth;
Step 4, by described polycrystal raw material powder, crystal pulling method or falling crucible method is adopted to be prepared into the described calcium fluoride crystal containing europium.
7., according to claim 6 containing the preparation method of europium calcium fluoride crystal, it is characterized in that, described falling crucible method comprises the following steps:
Step one, the plumbous fluoride that described polycrystal raw material powder adds 1 ~ 2wt% is mixed after put into plumbago crucible, described plumbago crucible is put into decline stove, and crystal growth direction is 100 or 111;
Step 2, vacuumize and make furnace interior vacuum tightness reach 1.0 × 10-
3more than Pa;
The lowering speed of step 3, described plumbago crucible is 1 ~ 2mm/h;
Step 4, temperature gradient of solid-liquid interface are about 20 DEG C/cm;
Be cooled to room temperature with the speed of 30 DEG C/h after step 5, crystal growth terminate, obtain the calcium fluoride crystal raw material containing europium;
Step 6, described crystal raw material carried out successively anneal, directed, cutting, grinding and polished finish, obtaining content range is mass percent 0.5 × 10
-3wt% ~ 5 × 10
-3the calcium fluoride crystal containing europium of wt%.
8., according to claim 6 containing the calcium fluoride crystal preparation method of europium, it is characterized in that, described crystal pulling method comprises the following steps:
Step one, the plumbous fluoride that described polycrystal raw material powder adds 1 ~ 2wt% is mixed after put into plumbago crucible, described plumbago crucible is put into decline stove, and crystal growth direction is 100 or 111;
Step 2, vacuumize and make furnace interior vacuum tightness reach 3.0 × 10
-3more than Pa, after be filled with argon gas and tetrafluoro-methane mixed gas as protective atmosphere;
Step 3, make crystal pull rate be 2 ~ 3mm/h, speed of rotation 20 ~ 30r/min, temperature gradient of solid-liquid interface is 10 DEG C/cm;
Room temperature is cooled to the speed of 30 DEG C/h after step 4, crystal growth terminate;
Step 5, above-mentioned crystal is annealed successively, directed, cutting, grinding and polished finish, obtaining content is mass percent 0.5 × 10
-3wt% ~ 5 × 10
-3the calcium fluoride crystal containing europium of wt%.
9. the calcium fluoride crystal purposes containing europium that according to claim 7 or 8 prepared by any one method, is characterized in that, the described calcium fluoride crystal containing europium is made into scintillation crystal.
10., according to claim 9 containing the calcium fluoride crystal purposes of europium, it is characterized in that, described scintillation crystal is made into scintillation crystal detectors.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105463568A (en) * | 2015-12-30 | 2016-04-06 | 哈尔滨工业大学 | Preparation method for holmium-doped yttrium barium fluoride crystals |
| CN106520115A (en) * | 2016-08-31 | 2017-03-22 | 佛山科学技术学院 | Water-soluble rare earth porous nano-crystal preparation method |
| CN108640686A (en) * | 2018-06-27 | 2018-10-12 | 武汉理工大学 | A kind of europium yttrium is co-doped with calcirm-fluoride scintillating ceramic and preparation method thereof |
| CN113173591A (en) * | 2021-03-09 | 2021-07-27 | 中国工程物理研究院材料研究所 | Calcium fluoride scintillation crystal particles for continuously measuring low-level radioactive nuclide in liquid effluent, and manufacturing process and device thereof |
| CN115818972A (en) * | 2022-11-16 | 2023-03-21 | 曹掌歧 | Glass scintillation substrate for detecting soft beta particle rays and preparation method thereof |
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| CN105463568A (en) * | 2015-12-30 | 2016-04-06 | 哈尔滨工业大学 | Preparation method for holmium-doped yttrium barium fluoride crystals |
| CN105463568B (en) * | 2015-12-30 | 2017-12-15 | 哈尔滨工业大学 | A kind of preparation method for mixing holmium yttrium fluoride crystal of barium |
| CN106520115A (en) * | 2016-08-31 | 2017-03-22 | 佛山科学技术学院 | Water-soluble rare earth porous nano-crystal preparation method |
| CN108640686A (en) * | 2018-06-27 | 2018-10-12 | 武汉理工大学 | A kind of europium yttrium is co-doped with calcirm-fluoride scintillating ceramic and preparation method thereof |
| CN113173591A (en) * | 2021-03-09 | 2021-07-27 | 中国工程物理研究院材料研究所 | Calcium fluoride scintillation crystal particles for continuously measuring low-level radioactive nuclide in liquid effluent, and manufacturing process and device thereof |
| CN115818972A (en) * | 2022-11-16 | 2023-03-21 | 曹掌歧 | Glass scintillation substrate for detecting soft beta particle rays and preparation method thereof |
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