CN102650076A - Method for growing lead chlorofluoride crystal and application of crystal produced by same - Google Patents
Method for growing lead chlorofluoride crystal and application of crystal produced by same Download PDFInfo
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- CN102650076A CN102650076A CN2011100472846A CN201110047284A CN102650076A CN 102650076 A CN102650076 A CN 102650076A CN 2011100472846 A CN2011100472846 A CN 2011100472846A CN 201110047284 A CN201110047284 A CN 201110047284A CN 102650076 A CN102650076 A CN 102650076A
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Abstract
The invention discloses a method for growing a lead chlorofluoride crystal, which is a non-vacuum Bridgman method, through adding deoxidizer into raw materials and adopting an airtight crucible and component proportioning control, the volatilization and oxidization problems of components during the growing process are fully solved, the problem that the lead chlorofluoride crystal is difficult to produce is also solved, the lead chlorofluoride crystal with large size and high quality is obtained, and the produced crystal can be applied in a radiation detection system. A structure which forms a Cerenkov and flare light double-reading radiation detection system is that: the lead chlorofluoride crystal is arranged between two photovoltaic conversion devices which are oppositely arranged and connected with the two photovoltaic conversion devices through filtering sheets which are arranged on the photovoltaic conversion devices, both the two photovoltaic conversion devices which are oppositely arranged are connected with a computer, and the lead chlorofluoride crystal is connected with the filtering sheets through silicone oil coupling. The method has the important meaning to not only the research of the lead chlorofluoride crystal but also the study of the radiation detection system.
Description
Technical field
The present invention relates to a kind of growth fluorine lead chloride crystalline method and this method gained crystalline uses; Specifically; Relate to a kind of utilize antivacuum crucible decline technology growth fluorine lead chloride crystalline method and the application of the prepared fluorine lead chloride of this method crystal in radiation detecting system, belong to the crystalline material technical field.
Background technology
Fluorine lead chloride (PbFCl) crystal made small pieces by J.Schoonman and G.J.Dirksen through horizontal zone-melting technique first in 1973.Fluorine lead chloride crystal has the following advantages: 1) have high-density (7.11g/cm
3); 2) have very short fall time (2.89ns and 23.42ns); 3) has stable chemical property, not deliquescence; 4) fluorine lead chloride crystalline ultraviolet absorption edge wavelength very short (270nm).2005, Chen Jianming reported that also fluorine lead chloride crystal at room temperature has scintillation properties.
Fluorine lead chloride crystal has shortcomings such as component is volatile, the easy oxidation of raw material, makes monocrystalline be difficult to preparation.General usage level float-zone method or Bridgman-Stockbarge method for growing fluorine lead chloride crystal are prone to component volatilization and oxidation when using these two kinds of method growing crystals in original technology, cause monocrystalline to be difficult to obtain, even obtain the fritter monocrystalline, crystal mass is also very poor.In addition, because fluorine lead chloride crystal is difficult to make, therefore, also do not see the relevant report that this crystal is used so far.
Summary of the invention
The present invention is directed to above-mentioned existing in prior technology defective and problem, the technical problem that solve provides a kind of growth fluorine lead chloride crystalline method and this method gained crystalline is used.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is following:
A kind of growth fluorine lead chloride crystalline method is antivacuum falling crucible method, comprises following concrete steps:
A) with PbF
2, PbCl
2Mix in proportion with reductor, wherein: PbF
2With PbCl
2Mol ratio be (0.8～1.2): 1; The quality of reductor is PbF
2With PbCl
23% of total mass;
B) material after above-mentioned the mixing is seated in the crucible, then sealed crucible;
C) crucible of sealing is put into crystal growing furnace, heating up then melts raw material;
D) adopt antivacuum Bridgman-Stockbarge method for growing crystal, crystal growth temperature is 650～800 ℃, and crystal growth rate is 0.1～2mm/h, and the thermograde of decline is 10～70 ℃/cm.
Said PbF
2And PbCl
2Material purity all be recommended as 99.99%.
Said reductor is the active substance with strong reducing action, is recommended as any one or a few the mixing in silicon carbide powder, bicarbonate of ammonia, ammonium sulphite, sulfurous acid ammonia, the lead sulfide.
Said crucible is the precious metal crucible; Be recommended as in platinum, iridium, ruthenium and the rhodium crucible any one; The shape of crucible is recommended as the special-shaped crucible of capillary or cone-shaped bottom, and mouth interior diameter, height and the thickness of crucible can be confirmed according to the crystalline size of required growth by those skilled in the art.
Said crystal growing furnace is two warm area crystal growing furnaces, comprises sleeve pipe, lagging material, heating member, thermal baffle, thermopair and following descending mechanism.
Said antivacuum being meant under the neutral atmosphere.
Size is big, the quality advantages of higher owing to the crystal that grows with the method for the invention has; When this crystal receives energetic ray and excites; Can launch Cherenkov's light and twinkling light simultaneously; Therefore; Can be used for Cherenkov's light and the two detecting materials of reading radiation detecting system of twinkling light by the prepared fluorine lead chloride of this method crystal, the two structures of reading radiation detecting system of Cherenkov's light of formation and twinkling light are: fluorine lead chloride crystal is located between two electrooptical devices of placing relatively, and is connected through the filter plate that is located on the electrooptical device; Two electrooptical devices of relatively placing all are connected with computingmachine, and being coupled through silicone oil between said fluorine lead chloride crystal and the filter plate is connected.
Said electrooptical device is recommended as PM or avalanche photodide.
The present invention can guarantee that through crucible sealing crucible crucible internal gas pressure when heating rises, and with effective inhibition feed composition volatilization, can also guarantee that the evaporable component can not overflow simultaneously in crucible.PbF among the present invention
2With PbCl
2Proportioning adopts non-stoichiometric, can guarantee component volatilization after, molten intravital PbF
2With PbCl
2Ratio is near stoichiometric ratio.The present invention can make the oxygen in the crucible react with it through adding reductor, in crucible, forms neutral atmosphere, fully avoids the influence of raw material oxidation to growing crystal.Further, the present invention adopts the special-shaped crucible of capillary or cone-shaped bottom, can guarantee that crystal carries out sufficient nucleation selection process when growth, further help the crystalline monocrystallineization.
Therefore; Compared with prior art; The present invention has fully solved component volatilization and the problem of oxidation in the process of growth through in raw material, adding reductor, adopting the airtight crucible and the control of set of dispense ratio, has solved the difficult problem that fluorine lead chloride crystal is difficult for making; Large size, high-quality fluorine lead chloride monocrystalline have been obtained; For two radiation detecting systems of reading provide a kind of ideal detecting material, not only significant to the research of fluorine lead chloride monocrystalline, also the research to radiation detecting system has important value.
Description of drawings
Fig. 1 is the structural representation of the crystal growing furnace described in the inventive method, among the figure: 1, sleeve pipe; 2, crucible; 3, heating member; 4, lagging material; 5, thermal baffle; 6, thermopair; 7, following descending mechanism.
Fig. 2 is the cross-sectional view of used crucible among the embodiment 1.
Fig. 3 is the cross-sectional view of used crucible among the embodiment 2.
Fig. 4 is the excitation of X-rays emission spectrum comparison diagram of fluorine lead chloride crystal and crystal of lead tungstate.
Fig. 5 is two structural representations of reading radiation detecting system of the present invention, among the figure: a, fluorine lead chloride crystal; B, electrooptical device; C, filter plate; D, computingmachine; E, energetic ray.
The practical implementation method
Below in conjunction with embodiment the present invention is done further in detail, intactly explains, but do not limit content of the present invention.
Embodiment 1
According to mol ratio is PbF
2: PbCl
2=49.5: 50.5 weighing PbF
2(purity is 99.99%) 46.36g, PbCl
2(purity is 99.99%) 53.64g adds reductor (silicon carbide powder) 3g, is seated in the point end crucible (its cross-sectional view is as shown in Figure 2) sealed crucible after mixing; The crucible of sealing is put into crystal growing furnace (its structural representation is as shown in Figure 1), and heating up then melts raw material; Adopt antivacuum Bridgman-Stockbarge method for growing crystal, crystal growth temperature is 650 ℃, and crystal growth rate is 1.5mm/h, and the thermograde of decline is 60 ℃/cm; Through 72 hours growth, can obtain 10 * 10 * 4mm
3About fluorine lead chloride monocrystalline, this crystalline flicker luminescent properties is as shown in Figure 4.
According to mol ratio is PbF
2: PbCl
2=50.5: 49.5, weighing PbF
2(purity is 99.99%) 47.35g, PbCl
2(purity is 99.99%) 52.65g adds reductor (silicon carbide powder 1.5g, bicarbonate of ammonia 1.5g) 3g, is seated at the bottom of the capillary in the crucible (its cross-sectional view is as shown in Figure 3) sealed crucible after mixing; The crucible of sealing is put into crystal growing furnace (its structural representation is as shown in Figure 1), and heating up then melts raw material; Adopt antivacuum Bridgman-Stockbarge method for growing crystal, crystal growth temperature is 680 ℃, and crystal growth rate is 1.5mm/h, and the thermograde of decline is 15 ℃/cm; Through 72 hours growth, can obtain diameter 15mm, the fluorine lead chloride monocrystalline about length 20mm, this crystalline flicker luminescent properties is as shown in Figure 4.
Embodiment 3
The two radiation detecting systems of reading of making Cherenkov's light as shown in Figure 5 and twinkling light: fluorine lead chloride crystal is located between two electrooptical devices of placing relatively; And be connected through the filter plate that is located on the electrooptical device; Two electrooptical devices of relatively placing all are connected with computingmachine, and being coupled through silicone oil between said fluorine lead chloride crystal and the filter plate is connected.
When said fluorine lead chloride crystal receives energetic ray and excites; This crystal can be launched Cherenkov's light and twinkling light simultaneously; The electrooptical device that is added with filter plate through use carries out the output of electrical signal, and this system can be through the two detections of reading the realization energetic ray to Cherenkov's light and twinkling light.
Said electrooptical device is recommended as PM or avalanche photodide.
Claims (10)
1. a growth fluorine lead chloride crystalline method is characterized in that, is antivacuum falling crucible method, comprises following concrete steps:
A) with PbF
2, PbCl
2Mix in proportion with reductor, wherein: PbF
2With PbCl
2Mol ratio be (0.8～1.2): 1; The quality of reductor is PbF
2With PbCl
23% of total mass;
B) material after above-mentioned the mixing is seated in the crucible, then sealed crucible;
C) crucible of sealing is put into crystal growing furnace, heating up then melts raw material;
D) adopt antivacuum Bridgman-Stockbarge method for growing crystal, crystal growth temperature is 650～800 ℃, and crystal growth rate is 0.1～2mm/h, and the thermograde of decline is 10～70 ℃/cm.
2. growth fluorine lead chloride crystalline method according to claim 1 is characterized in that: PbF
2And PbCl
2Material purity be 99.99%.
3. growth fluorine lead chloride crystalline method according to claim 1 is characterized in that: said reductor is selected from any one or a few the mixing in silicon carbide powder, bicarbonate of ammonia, ammonium sulphite, sulfurous acid ammonia, the lead sulfide.
4. growth fluorine lead chloride crystalline method according to claim 1, it is characterized in that: said crucible is any one in platinum, iridium, ruthenium and the rhodium crucible.
5. growth fluorine lead chloride crystalline method according to claim 1 is characterized in that: the special-shaped crucible that is shaped as capillary or cone-shaped bottom of said crucible.
6. growth fluorine lead chloride crystalline method according to claim 1 is characterized in that: said crystal growing furnace comprises sleeve pipe, lagging material, heating member, thermal baffle, thermopair and following descending mechanism for two warm area crystal growing furnaces.
7. growth fluorine lead chloride crystalline method according to claim 1 is characterized in that: said antivacuum being meant under the neutral atmosphere.
8. the resulting fluorine lead chloride of each said method crystalline is used in the claim 1 to 7, it is characterized in that: be used for the detecting materials that Cherenkov's light and twinkling light pair are read radiation detecting system.
9. fluorine lead chloride crystalline according to claim 8 is used; It is characterized in that: fluorine lead chloride crystal is located between two electrooptical devices of placing relatively; And be attached thereto and connect through being located at filter plate on the electrooptical device; Two electrooptical devices of relatively placing all are connected with computingmachine, be connected through the silicone oil coupling between said fluorine lead chloride crystal and the filter plate, thereby formation Cherenkov's light and twinkling light pair are read radiation detecting systems.
10. fluorine lead chloride crystalline according to claim 9 is used, and it is characterized in that: said electrooptical device is PM or avalanche photodide.
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|---|---|---|---|
| CN2011100472846A CN102650076A (en) | 2011-02-28 | 2011-02-28 | Method for growing lead chlorofluoride crystal and application of crystal produced by same |
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|---|---|---|---|
| CN2011100472846A CN102650076A (en) | 2011-02-28 | 2011-02-28 | Method for growing lead chlorofluoride crystal and application of crystal produced by same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113031044A (en) * | 2019-12-25 | 2021-06-25 | 同方威视技术股份有限公司 | Detector and detection device for radiation inspection |
Citations (5)
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|---|---|---|---|---|
| PL148277B1 (en) * | 1986-11-24 | 1989-09-30 | Method of obtaining crystalline lanthanum chloride of particulary high purity | |
| CN1113970A (en) * | 1994-06-23 | 1995-12-27 | 中国科学院上海硅酸盐研究所 | Descent method for growing large size cesium iodide (CSI) crystal |
| US20050082484A1 (en) * | 2003-10-17 | 2005-04-21 | Srivastava Alok M. | Scintillator compositions, and related processes and articles of manufacture |
| CN1793439A (en) * | 2005-11-25 | 2006-06-28 | 中国科学院上海硅酸盐研究所 | Process for growing lanthanum chloride crystal by falling method of antivacuum crucible |
| CN1800092A (en) * | 2005-05-13 | 2006-07-12 | 中国科学院上海硅酸盐研究所 | Hafnium oxide-gadolinium oxide solid solution transparent ceramic glaring material and its preparation method and uses |
-
2011
- 2011-02-28 CN CN2011100472846A patent/CN102650076A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PL148277B1 (en) * | 1986-11-24 | 1989-09-30 | Method of obtaining crystalline lanthanum chloride of particulary high purity | |
| CN1113970A (en) * | 1994-06-23 | 1995-12-27 | 中国科学院上海硅酸盐研究所 | Descent method for growing large size cesium iodide (CSI) crystal |
| US20050082484A1 (en) * | 2003-10-17 | 2005-04-21 | Srivastava Alok M. | Scintillator compositions, and related processes and articles of manufacture |
| CN1800092A (en) * | 2005-05-13 | 2006-07-12 | 中国科学院上海硅酸盐研究所 | Hafnium oxide-gadolinium oxide solid solution transparent ceramic glaring material and its preparation method and uses |
| CN1793439A (en) * | 2005-11-25 | 2006-06-28 | 中国科学院上海硅酸盐研究所 | Process for growing lanthanum chloride crystal by falling method of antivacuum crucible |
Non-Patent Citations (3)
| Title |
|---|
| BO LIU,ETAL: "Luminescence spectra of PbFCl single crystal under the excitation of synchrotron radiation VUV–UV", 《JOURNAL OF LUMINESCENCE》 * |
| JIANMING CHEN,ETAL: "Study of effects of F/Cl ratio on crystal growth and X-ray excited luminescence of PbFCl", 《JOURNAL OF CRYSTAL GROWTH》 * |
| 陈建明: "氟氯化铅晶体生长及闪烁性能研究", 《中国科学院上海硅酸盐研究所博士学位论文》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113031044A (en) * | 2019-12-25 | 2021-06-25 | 同方威视技术股份有限公司 | Detector and detection device for radiation inspection |
| CN113031044B (en) * | 2019-12-25 | 2024-01-19 | 同方威视技术股份有限公司 | Detector and detection device for radiation inspection |
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Application publication date: 20120829 |