CN105293943A - Glass film containing rare-earth-ion-doped lithium iodide microcrystalline and preparation method thereof - Google Patents
Glass film containing rare-earth-ion-doped lithium iodide microcrystalline and preparation method thereof Download PDFInfo
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Abstract
A disclosed glass film containing rare-earth-ion-doped lithium iodide microcrystalline is characterized in that the glass film comprises the following compositions in percent by mole: 76-79 mol% of germanium oxide, 8-12 mol% of niobium pentoxide, 8-12 mol% of lithium iodide, and 1-4 mol% of a rare-earth iodide, wherein the rare-earth iodide is one of cerium iodide, europium iodide and terbium iodide. The advantages comprise that a sol-gel technology is a low-temperature wet-chemical-process glass preparation technology, the glass is obtained through hydrolysis of a precursor raw material and a polymerization chemical reaction process, the film material can be prepared under a certain liquid viscosity condition, and the low-temperature synthesis condition is capable of effectively preventing the iodide raw material from being decomposed and volatilized; and because of volatilization and decomposition of the solvent, certain micropores are generated in the glass prepared through the sol-gel method, and the micropores provide good environment for generation of nanometer iodide microcrystalline, and thus crystallized-particle nonuniformity and glass devitrificationcaused by incomplete uniformity of melt-glass chemical compositions and crystallization processing temperature are overcome to a certain degree.
Description
Technical field
The present invention relates to a kind of glass film of rare earth ion doped crystallite, be specifically related to a kind of glass film and the process for preparing sol-gel thereof that are used as rare earth ion doped lithium iodide (LiI) crystallite of scintillation material.
Background technology
Scintillation material is a kind of lower optical function material that can send visible ray of exciting at energetic ray (as x-ray, gamma-rays) or other radioactive particle, can be widely used in nuclear medicine diagnostic, safety check, anti-ly to fear, the field such as high energy physics and geological prospecting.In recent years along with the fast development in the field such as medical imaging and safety inspection, the high performance new scintillation material of demand in large quantities.Outstanding scintillation material mainly possesses following performance: luminous efficiency is high, density of material is large, fluorescence decay is fast, radiation resistance is good and the low inferior feature of production cost.
With regard to current scintillation material, primarily of single crystal and glass bi-material.Scintillating monocrystal has the advantage such as resistance to irradiation, fast decay, High Light Output usually, but it exists that technique preparation is complicated, cost value is expensive and the shortcoming such as large size single crystal body difficulty acquisition.What is more, and be doped in rare earth luminous ion in single crystal owing to there is Segregation, the distribution in crystal is very uneven, therefore seriously affects the rate of utilization of its luminescent properties and material.Scintillation glass possess rear-earth-doped evenly, the feature such as cost is low, large-size glass is easy to preparation, chemical composition easily regulates, but its aspect such as light output, multiplicity performance is inferior to single crystal usually, and therefore its application is also severely limited.
Lithium iodate crystal is a kind of flicker substrate material of excellence, Ce
3+the lithium iodate crystal of doping has abnormal high light output, and good energy resolution, can be applicable in low energy physics and the field such as safety check, medical imaging.Eu
3+, Tb
3+the lithium iodate crystal of doping also has High Light Output, and the feature of fast decay, can be used for the fields such as scintillation fluor screen.But lithium iodate crystal is deliquescence, poor, the easy cleavage slabbing of mechanical property, its practical application of the large-size crystals growth disadvantages affect such as difficult, expensive very easily.
Notification number is the patent of invention of CN103951224A, then disclose by high temperature melting legal system for P
2o
5-GeO
2-NaF-Li
2o-LiI-LnI
3system glass, then by being incubated near glass transition temperature, separates out rare earth ion doped lithium iodide crystallite, is prepared into the rare earth ion doped lithium iodide devitrified glass of collection glass and single crystal performance.But there is following defect in the method, first: because at high temperature melting obtains, therefore easily cause the decomposition of iodide raw material; Second: its chemical composition of glass of preparation and the incomplete homogeneity of crystallization holding temperature usually, the microcrystallite size of precipitation is very uneven, very easily causes the devitrification of glass; 3rd: in Crystallization Process, in the lattice position of rare earth luminous ion lithium iodide difficult to get access, affect the illumination effect of material.In addition, due to high temperature melting method glass preparation technique, the glass of production is block, is difficult to the material obtaining thin-film state.Along with extensively popularizing of civil nature, small-sized, integrated flash device is the road of the certainty of Future Development.Usual film and fibrous material are the most suitable starting material making such device, and the development of therefore current scintillation material form to device from now on can produce larger restriction.
Summary of the invention
The technical problem to be solved in the present invention is to provide that a kind of physical and chemical performance is stable, physical strength is high, Deliquescence-resistant is strong, optical transmission is high, content of crystallite is high, there is glass film containing rare earth ion doped lithium iodide crystallite of high light output, soon decay and good energy resolution and temporal resolution characteristic and preparation method thereof simultaneously, this film physical and chemical performance is good, and preparation method has that equipment is simple, production cost is lower, easy to operate, combined coefficient is high, the crystallite size in the glass film of synthesis evenly, the doping content of degree of crystallinity and rare earth ion is high.
The present invention solves the problems of the technologies described above adopted technical scheme: containing the glass film of rare earth ion doped lithium iodide crystallite, its Mole percent consists of: germanium oxide: 76-79mol%, Niobium Pentxoxide: 8-12%, lithium iodide: 8-12mol%, rare-earth iodide: 1-4mol%, and wherein rare-earth iodide is the one in cerous iodide, iodate europium, iodate terbium.
2. the preparation method of the glass film containing rare earth ion doped lithium iodide crystallite according to claim 1, is characterized in that comprising following concrete steps:
The preparation of raw material:
(1), by raw materials in molar ratio: tetraethoxy germanium: ethanol niobium: lithium iodide: rare-earth iodide=76-79: 16-24: 8-12: 1-4, take analytically pure each raw materials respectively, rare-earth iodide is the one in cerous iodide, iodate europium, iodate terbium, stand-by; Lithium iodide, cerous iodide, iodate europium can replace with the iodide of other crystal water of identical mole with iodate terbium.
The preparation method of the described glass film containing rare earth ion doped lithium iodide crystallite, comprises following concrete steps:
The preparation of gel:
(2), the hydrolysis of tetraethoxy germanium: the tetraethoxy germanium of weighing in step (1) is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and tetraethoxy germanium is 2.5: 1, add methyl ethyl diketone fast, the volume ratio of tetraethoxy germanium and methyl ethyl diketone is 0.8: 1, and carry out the stirring of strong magnetic power, progressively instill distilled water, the mol ratio of distilled water and tetraethoxy germanium is 0.8: 1, regulate its pH value to 4 ~ 5 with concentrated nitric acid, be hydrolyzed under room temperature reaction 1 hour, makes solution A;
(3), the hydrolysis of ethanol niobium: the ethanol niobium of weighing in step (1) is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and ethanol niobium is 2.5: 1, add methyl ethyl diketone fast, the volume ratio of ethanol niobium and methyl ethyl diketone is 1: 1, and carries out the stirring of strong magnetic power, progressively instills distilled water, the mol ratio of distilled water and ethanol niobium is 0.6: 1, regulate its pH value to 4 ~ 5 with concentrated nitric acid, be hydrolyzed under room temperature reaction 1 hour, makes solution B;
(4), by solution B slowly join in solution A, after abundant mix and blend, then drip a certain amount of distilled water, carry out secondary hydrolysis reaction, the mol ratio of distilled water and tetraethoxy germanium, both ethanol niobiums summation is 0.6: 1, and mixed hydrolysis makes solution C after reacting 0.5 hour;
(5), in solution C, add the measured lithium iodide of scale and rare-earth iodide in step (1), under vigorous stirring, hydrolysis reaction, after 2 hours, makes solution D;
(6), by after solution D sealing leave standstill 1 day, obtain the solution E of certain viscosity;
The preparation of film:
(7), solution E dip-coating method (dip-coating) is coated on clean glass substrate, the pull rate of glass substrate in gelating soln controls in 0.2-1 mm/second, lift 1-5 time can be repeated according to concrete thickness requirement, each lift interval time is 15 minutes, and the film after coating at room temperature dries 4 hours;
The thermal treatment of film:
(8), the film that step (7) is obtained is placed in stove, with the ramp of 30-50 per hour DEG C to 100 DEG C, be incubated 1 hour, to remove remaining water and ethanol, then heat up stove again to 340 DEG C with the speed of 30-50 per hour DEG C, be incubated 20 minutes, to remove organism remaining in film, thermal treatment terminates, and with 50 DEG C of rate of temperature fall per hour, Slow cooling stove is to room temperature;
The hydrogen iodide high temperature Crystallizing treatment of film:
(9), the film that step (8) obtains is put into the quartz pipe of tube type resistance furnace, first the air in quartz pipe is got rid of with nitrogen, then hydrogen iodide cylinder valve is opened, pass into dry hydrogen iodide gas, with the speed of 50 DEG C per hour, progressively intensification stove is to 360-380 DEG C, and reaction treatment 1-3 hour at such a temperature, reaction treatment terminates, close hydrogen iodide gas, and with 50 DEG C of rate of temperature fall per hour, Slow cooling tube type resistance furnace is to room temperature, with hydrogen iodide gas residual in nitrogen purge pipeline, all remaining iodate hydrogen through pipeline tail end is reclaimed by sodium hydroxide solution, finally obtain the glass film containing rare earth ion doped lithium iodide crystallite.This preparation method has that equipment is simple, production cost is lower, easy to operate, combined coefficient is high, and the crystallite size in the glass film of synthesis evenly, the doping content of degree of crystallinity and rare earth ion is high.
In described step (1), raw materials is made up of according to following mol ratio following substances: tetraethoxy germanium: ethanol niobium: lithium iodide: cerous iodide=79: 24: 8: 1.
In described step (1), raw materials is made up of according to following mol ratio following substances: tetraethoxy germanium: ethanol niobium: lithium iodide: iodate europium=76: 16: 12: 4.
In described step (1), raw materials is made up of according to following mol ratio following substances: tetraethoxy germanium: ethanol niobium: lithium iodide: iodate terbium=78: 20: 10: 2.
Compared with prior art, advantage of the present invention is:
1, sol-gel is a kind of Low Temperature Wet chemical method glass making techniques, obtains glass, therefore can be prepared into thin-film material under certain liquid viscosity by the hydrolysis of precursor raw material and polymeric chemical reaction process.
2, the synthesis condition of low temperature can prevent decomposition and the volatilization of iodide raw material effectively.
3, the glass prepared of sol-gel method is due to the volatilization of solvent and decomposition, certain micropore can be generated in the material, the environment that the generation that these micropores are nanometer iodide crystallite provides, thus the incomplete homogeneity of the chemical composition that can to a certain degree overcome due to fusion cast glass and crystallization treatment temp, cause the devitrification of the uneven of crystallization particle and glass.
4, as rare earth and the Li of glass network modifier
+ion, most one is in together in micropore gap, and therefore along with the carrying out of high temperature hydrogen iodide process, rare earth luminous ion easily enters in the lattice position of lithium iodide, obtains the rare earth ion doped and illumination effect of high density.
5, the hydrogen iodide drying treatment of high temperature impels iodine Lithium Oxide 98min, lithium hydroxide and Lithium Oxide 98min etc. in gel glass to convert lithium iodide to, can carry out the dehydration reaction of iodide raw material, and effectively promotes and the generation controlling calcium iodide lithium crystalline substance.
Because this film glass matrix is GeO
2-Nb
2o
5two-phase system, therefore can change optics and physical and chemical performance that original one-tenth assigns to regulate film according to the actual requirements.This film is high in the transmitance of ultraviolet band, according to the actual requirements, alterable component is equipped with and regulates its physical and chemical performance and optical property, containing the germanium niobate glass film material of rare earth ion doped lithium iodide crystallite, there is superior scintillation properties, physical strength, thermal stability characteristics, the shortcoming such as overcome lithium iodide single crystal very easily deliquescence, mechanical property be poor; The experiment proved that: by formula of the present invention and preparation method, separate out rare earth ion doped lithium iodide crystalline phase, obtained ion doping lithium iodide devitrified glass is transparent, energy Deliquescence-resistant, good mechanical property, short wavelength's royal purple light transmission rate are higher, there is extremely strong light output, fast decay, the performances such as good energy resolution and temporal resolution, can make scintillation detectors efficiency increase substantially.This thin-film material is that the development of small-sized flash device from now on provides material base.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) figure of glass film after embodiment monoiod(in)ate hydrogen high temperature Crystallizing treatment;
Fig. 2 be embodiment one excitation of X-rays containing Ce
3+the fluorescence spectrum of the glass film of ion doping lithium iodide crystallite;
Fig. 3 be embodiment two excitation of X-rays containing Eu
3+the fluorescence spectrum of the glass film of ion doping lithium iodide crystallite;
Fig. 4 be embodiment three excitation of X-rays containing Tb
3+the fluorescence spectrum of the glass film of ion doping lithium iodide crystallite.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment one
Containing the preparation method of the glass film of rare earth ion doped lithium iodide crystallite, comprise following concrete steps:
(1) by raw materials in molar ratio: tetraethoxy germanium: ethanol niobium: lithium iodide: cerous iodide=79: 24: 8: 1, analytically pure each raw materials that total amount is 20 grams is taken, stand-by;
(2), the hydrolysis of tetraethoxy germanium: the tetraethoxy germanium of weighing in step (1) is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and tetraethoxy germanium is 2.5: 1, add methyl ethyl diketone fast, the volume ratio of tetraethoxy germanium and methyl ethyl diketone is 0.8: 1, and carry out the stirring of strong magnetic power, progressively instill distilled water, the mol ratio of distilled water and tetraethoxy germanium is 0.8: 1, regulate its pH value to 4 ~ 5 with concentrated nitric acid, be hydrolyzed under room temperature reaction 1 hour, makes solution A;
(3), the hydrolysis of ethanol niobium: the ethanol niobium of weighing in step (1) is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and ethanol niobium is 2.5: 1, add methyl ethyl diketone fast, the volume ratio of ethanol niobium and methyl ethyl diketone is 1: 1, and carries out the stirring of strong magnetic power, progressively instills distilled water, the mol ratio of distilled water and ethanol niobium is 0.6: 1, regulate its pH value to 4-5 with concentrated nitric acid, be hydrolyzed under room temperature reaction 1 hour, makes solution B;
(4), by solution B slowly join in solution A, after abundant mix and blend, then drip a certain amount of distilled water, carry out secondary hydrolysis reaction, the mol ratio of distilled water and tetraethoxy germanium, both ethanol niobiums summation is 0.6: 1, and mixed hydrolysis makes solution C after reacting 0.5 hour;
(5), in solution C, add the measured lithium iodide of scale and cerous iodide in step (1), under vigorous stirring, hydrolysis reaction, after 2 hours, makes solution D; (6), by the mixed sols solution D generated after sealing, leave standstill 1 day, obtain the vitreosol solution E of certain viscosity;
(7), solution E dip-coating method (dip-coating) is coated on clean glass substrate, the pull rate of glass substrate in gelating soln controls in 0.2-1 mm/second, lift 1-5 time can be repeated according to concrete thickness requirement, each lift interval time is 15 minutes, and the film after coating at room temperature dries 4 hours;
(8), the film that step (7) is obtained is placed in stove, with the ramp of 30 DEG C per hour to 100 DEG C, be incubated 1 hour, to remove remaining water and ethanol, then heat up stove again to 340 DEG C with the speed of 30 DEG C per hour, be incubated 20 minutes, to remove organism remaining in film, thermal treatment terminates, and with 50 DEG C of rate of temperature fall per hour, Slow cooling stove is to room temperature;
(9), the film that step (8) obtains is put into the quartz pipe of tube type resistance furnace, first the air in quartz pipe is got rid of with nitrogen, then hydrogen iodide cylinder valve is opened, pass into dry hydrogen iodide gas, with the speed of 50 DEG C per hour, progressively intensification stove is to 360 DEG C, and reaction treatment 3 hours at such a temperature, reaction treatment terminates, close hydrogen iodide gas, and with 50 DEG C of rate of temperature fall per hour, Slow cooling tube type resistance furnace is to room temperature, with hydrogen iodide gas residual in nitrogen purge pipeline, all remaining iodate hydrogen through pipeline tail end is reclaimed by sodium hydroxide solution, finally obtain containing Ce
3+the glass film of ion doping lithium iodide crystallite, the glass film molar constituent of acquisition is: 79GeO
2-12Nb
2o
5-8LiI-1CeI
3.
Ce is contained to what prepare
3+the glass film of ion doping lithium iodide crystallite carries out performance test, scrape and collect film powder, the XRD figure of glass thin coating materials after hydrogen iodide process as shown in Figure 1, its result is as follows: all conform to the main diffraction peak of the standard x RD figure of lithium iodide crystalline phase through processing the XRD diffraction peak of sample obtained, and what therefore obtain is the glass film containing lithium iodide crystallite.The Ce of excitation of X-rays
3+as shown in Figure 2, with compared with hydrogen iodide Crystallizing treatment, fluorescence intensity significantly strengthens the fluorescence spectrum of ion doping lithium iodide devitrified glass film, and fluorescence decay time is 54ns.
Embodiment two
Substantially identical with embodiment one, difference is that in step (1), raw materials is according to following mol ratio: tetraethoxy germanium: ethanol niobium: lithium iodide: iodate europium=76: 16: 12: 4, takes each raw materials respectively; In step (7), the pull rate of glass substrate in gelating soln controls in 1 mm/second, repeats lift 5 times, and lift interval time is 15 minutes at every turn; In step (8), with the ramp of 50 DEG C per hour to 100 DEG C, then heat up stove again to 340 DEG C with the speed of 50 DEG C per hour; In step (9), progressively intensification stove is to 380 DEG C, and reaction treatment 1 hour at such a temperature, the glass film molar constituent of acquisition is: 76GeO
2-8Nb
2o
5-12LiI-4EuI
3.
Eu is contained to what prepare
3+the glass film of ion doping lithium iodide crystallite carries out performance test, and the XRD figure of glass film after hydrogen iodide process is substantially identical with Fig. 1, and just intensity is different, and what therefore obtain is the glass film containing lithium iodide crystallite.The Eu of excitation of X-rays
3+as shown in Figure 3, with compared with hydrogen iodide Crystallizing treatment, fluorescence intensity significantly strengthens the fluorescence spectrum of the glass film of ion doping iodate crystallite.
Embodiment three
Substantially identical with embodiment one, difference is that in step (1), raw materials is according to following mol ratio: tetraethoxy germanium: ethanol niobium: lithium iodide: iodate terbium=78: 20: 10: 2, takes each raw materials respectively; In step (7), the pull rate of glass substrate in gelating soln controls in 0.6 mm/second, repeats lift 3 times, and lift interval time is 15 minutes at every turn; In step (8), with the ramp of 40 DEG C per hour to 100 DEG C, then heat up stove again to 340 DEG C with the speed of 40 DEG C per hour; In step (10), progressively intensification stove is to 370 DEG C, and reaction treatment 2 hours at such a temperature, the glass film molar constituent of acquisition is: 78GeO
2-10Nb
2o
5-10LiI-2TbI
3.
Tb is contained to what prepare
3+the glass film of ion doping lithium iodide crystallite carries out performance test, and the XRD figure of glass film after hydrogen iodide process is substantially identical with Fig. 1, and just intensity is different, and what therefore obtain is the glass film containing lithium iodide crystallite.The Tb of excitation of X-rays
3+as shown in Figure 4, with compared with hydrogen iodide Crystallizing treatment, fluorescence intensity significantly strengthens the fluorescence spectrum of the glass film of ion doping lithium iodide crystallite.
Claims (5)
1. containing the glass film of rare earth ion doped lithium iodide crystallite, it is characterized in that its Mole percent consists of: germanium oxide: 76-79mol%, Niobium Pentxoxide: 8-12%, lithium iodide: 8-12mol%, rare-earth iodide: 1-4mol%, wherein rare-earth iodide is the one in cerous iodide, iodate europium or iodate terbium.
2. the preparation method of the glass film containing rare earth ion doped lithium iodide crystallite according to claim 1, is characterized in that comprising following concrete steps:
(1), by raw materials in molar ratio: tetraethoxy germanium: ethanol niobium: lithium iodide: rare-earth iodide=76-79: 16-24: 8-12: 1-4, analytically pure each raw materials is taken respectively, stand-by;
(2), the hydrolysis of tetraethoxy germanium: the tetraethoxy germanium of weighing in step (1) is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and tetraethoxy germanium is 2.5: 1, add methyl ethyl diketone fast, the volume ratio of tetraethoxy germanium and methyl ethyl diketone is 0.8: 1, and carry out the stirring of strong magnetic power, progressively instill distilled water, the mol ratio of distilled water and tetraethoxy germanium is 0.8: 1, regulate its pH value to 4-5 with concentrated nitric acid, be hydrolyzed under room temperature reaction 1 hour, makes solution A;
(3), the hydrolysis of ethanol niobium: the ethanol niobium of weighing in step (1) is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and ethanol niobium is 2.5: 1, add methyl ethyl diketone fast, the volume ratio of ethanol niobium and methyl ethyl diketone is 1: 1, and carries out the stirring of strong magnetic power, progressively instills distilled water, the mol ratio of distilled water and ethanol niobium is 0.6: 1, regulate its pH value to 4-5 with concentrated nitric acid, be hydrolyzed under room temperature reaction 1 hour, makes solution B;
(4), by solution B slowly join in solution A, after abundant mix and blend, then drip a certain amount of distilled water, carry out secondary hydrolysis reaction, the mol ratio of distilled water and tetraethoxy germanium, both ethanol niobiums summation is 0.6: 1, and mixed hydrolysis makes solution C after reacting 0.5 hour;
(5), in solution C, add lithium iodide and the rare-earth iodide of weighing in step (1), under vigorous stirring, hydrolysis reaction, after 2 hours, makes solution D;
(6), by after solution D sealing leave standstill 1 day, obtain the solution E of certain viscosity;
(7), solution E dip-coating method is coated on clean glass substrate, the pull rate of glass substrate in solution E controls in 0.2-1 mm/second, lift 1-5 time can be repeated according to concrete thickness requirement, each lift interval time is 15 minutes, and the film after coating at room temperature dries 4 hours;
(8), the film that step (7) is obtained is placed in stove, with the ramp of 30-50 per hour DEG C to 100 DEG C, be incubated 1 hour, to remove remaining water and ethanol, then heat up stove again to 340 DEG C with the speed of 30-50 per hour DEG C, be incubated 20 minutes, to remove organism remaining in film, thermal treatment terminates, and with 50 DEG C of rate of temperature fall per hour, Slow cooling stove is to room temperature;
(9), the film that step (8) obtains is put into the quartz pipe of tube type resistance furnace, first the air in quartz pipe is got rid of with nitrogen, then hydrogen iodide cylinder valve is opened, pass into dry hydrogen iodide gas, with the speed of 50 DEG C per hour, progressively intensification stove is to 360-380 DEG C, and reaction treatment 1-3 hour at such a temperature, reaction treatment terminates, close hydrogen iodide gas, and with 50 DEG C of rate of temperature fall per hour, Slow cooling tube type resistance furnace is to room temperature, with hydrogen iodide gas residual in nitrogen purge pipeline, all remaining iodate hydrogen through pipeline tail end is reclaimed by sodium hydroxide solution, finally obtain the glass film containing rare earth ion doped lithium iodide crystallite.
3. the glass film containing rare earth ion doped lithium iodide crystallite as claimed in claim 2, it is characterized in that in described step (1), raw materials is made up of according to following mol ratio following substances: tetraethoxy germanium: ethanol niobium: lithium iodide: cerous iodide=79: 24: 8: 1.
4. the glass film containing rare earth ion doped lithium iodide crystallite as claimed in claim 2, it is characterized in that in described step (1), raw materials is made up of according to following mol ratio following substances: tetraethoxy germanium: ethanol niobium: lithium iodide: iodate europium=76: 16: 12: 4.
5. the glass film containing rare earth ion doped lithium iodide crystallite as claimed in claim 2, it is characterized in that in described step (1), raw materials is made up of according to following mol ratio following substances: tetraethoxy germanium: ethanol niobium: lithium iodide: iodate terbium=78: 20: 10: 2.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024553A (en) * | 2006-02-24 | 2007-08-29 | 中国科学院福建物质结构研究所 | Alkaline-earth contained fluoride nano crystal transparent glass ceramic and its sol-gel preparing method |
| US20080241040A1 (en) * | 2007-03-26 | 2008-10-02 | General Electric Company | Nano-scale metal halide scintillation materials and methods for making same |
| CN1651548B (en) * | 2004-02-06 | 2010-06-16 | 乌克兰国家科学研究院闪烁物质研究所 | Scintillating material based on doped lithium iodide |
| CN102517002A (en) * | 2011-12-06 | 2012-06-27 | 中国科学院福建物质结构研究所 | Preparation method for alkaline earth fluo-chloride up-conversion luminescence nanometer crystal |
| CN103951224A (en) * | 2014-05-08 | 2014-07-30 | 宁波大学 | Rare-earth-ion-doped LiI microcrystalline glass and preparation method thereof |
-
2015
- 2015-11-16 CN CN201510783067.1A patent/CN105293943A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1651548B (en) * | 2004-02-06 | 2010-06-16 | 乌克兰国家科学研究院闪烁物质研究所 | Scintillating material based on doped lithium iodide |
| CN101024553A (en) * | 2006-02-24 | 2007-08-29 | 中国科学院福建物质结构研究所 | Alkaline-earth contained fluoride nano crystal transparent glass ceramic and its sol-gel preparing method |
| US20080241040A1 (en) * | 2007-03-26 | 2008-10-02 | General Electric Company | Nano-scale metal halide scintillation materials and methods for making same |
| CN102517002A (en) * | 2011-12-06 | 2012-06-27 | 中国科学院福建物质结构研究所 | Preparation method for alkaline earth fluo-chloride up-conversion luminescence nanometer crystal |
| CN103951224A (en) * | 2014-05-08 | 2014-07-30 | 宁波大学 | Rare-earth-ion-doped LiI microcrystalline glass and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| 李龙等: "《检验核医学》", 30 June 2009, 东南大学出版社 * |
| 游首先等: "《兵器工业科学技术辞典光学工程》", 31 May 1993, 国防工业出版社 * |
| 陈红兵等: "CuI微晶掺杂硅凝胶玻璃及其薄膜的制备", 《材料研究学报》 * |
| 黄剑锋: "《溶胶凝胶原理与技术》", 30 September 2005, 化学工业出版社 * |
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