CN105293941A - Preparation method for glass film containing divalent-europium-ion-doped strontium iodide microcrystalline - Google Patents
Preparation method for glass film containing divalent-europium-ion-doped strontium iodide microcrystalline Download PDFInfo
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Abstract
The invention discloses a preparation method for a glass film containing divalent-europium-ion-doped strontium iodide microcrystalline. The preparation method is characterized in that the preparation raw materials comprises, in percent by mole, 65-74 mol% of ethyl orthosilicate, 5-10 mol% of aluminium tri-sec-butoxide, 5-10 mol% of tributyl borate, 10-16 mol% of strontium iodide, and 1-4 mol% of europium(II) 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 devitrification caused 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 technology of preparing of glass film of rare earth ion doped crystallite, be specifically related to a kind of be used as scintillation material containing divalent europium (Eu
2+) doping strontium iodide (SrI
2) process for preparing sol-gel of glass film of crystallite.
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.
Europium ion presents+2 and+3 two kinds of valence states usually, under the exciting of X-ray, divalent europium has fluorescent emission faster than trivalent europium ion, and therefore centered by divalent europium, the scintillation material of light emitting ionic is expected to have higher resolving power, may be used on special flicker field.The research in past shows, strontium iodide crystal is a kind of flicker substrate material of excellence, it is high that rare earth ion doped strontium iodide crystal has light output, fast decay, good energy resolution, temporal resolution and linear response, have than rare earth ion doped crystal of fluoride and the higher luminous efficiency of oxide crystal, scintillation detectors efficiency can be made to increase substantially.Because divalent europium and strontium ion have analogous ionic radius size and identical ionic valence condition, the divalent europium of more amount of can adulterating, thus obtain the high resolution device based on divalent europium doping strontium iodide material.But the defects such as poor, the easy cleavage of strontium iodide host crystal mechanical property and very easily deliquescence, and large-size crystals grows its practical applications of disadvantages affect such as difficult and expensive.
Notification number is the patent of invention of CN103951258A, then disclose by high temperature melting legal system for B
2o
3-BaF
2-NaF-SrO-SrI
2-EuI
2system glass, then by being incubated near glass transition temperature, separating out the strontium iodide crystallite of divalent europium doping, being prepared into the rare earth ion doped strontium 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 strontium 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 the preparation method of devitrified glass film of the strontium iodide that adulterates containing divalent europium of high light output, fast decay and good energy resolution and temporal resolution characteristic simultaneously, 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.
The present invention solves the problems of the technologies described above adopted technical scheme: containing the preparation method of the glass film of divalent europium doped microcrystalline, comprise the steps:
The preparation of raw material:
(1), raw materials is pressed mole percentage composition: tetraethoxy: 65-74mol%, aluminium secondary butylate: 5-10mol%, tri-n-butyl borate: 5-10mol%, strontium iodide: 10-16mol%, sub-europium: the 1-4mol% of iodate, take analytically pure each raw materials respectively, stand-by; Strontium iodide can replace with the iodide of other crystal water of identical mole with the sub-europium of iodate;
The preparation of gel:
(2), the hydrolysis of aluminium secondary butylate: the aluminium secondary butylate of weighing in step (1) is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and aluminium secondary butylate is 3: 1, add Glacial acetic acid fast, using as sequestrant, effectively can contain the hydrolysis reaction of aluminium secondary butylate, the volume ratio of aluminium secondary butylate and Glacial acetic acid is 1: 1, and carry out the stirring of strong magnetic power, progressively instill distilled water, the mol ratio of distilled water and aluminium secondary butylate is 1: 1, be hydrolyzed under room temperature reaction 1 hour, makes solution A;
(3), the hydrolysis of tri-n-butyl borate: the tri-n-butyl borate of weighing in step (1) is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and tri-n-butyl borate is 2.5: 1, add Glacial acetic acid fast, using as sequestrant, effectively can contain the hydrolysis reaction of tri-n-butyl borate, the volume ratio of tri-n-butyl borate and Glacial acetic acid is 1: 1, and carry out the stirring of strong magnetic power, progressively instill distilled water, the mol ratio of distilled water and tri-n-butyl borate is 0.8: 1, be hydrolyzed under room temperature reaction 1 hour, makes solution B;
(4), the hydrolysis of tetraethoxy: the measured tetraethoxy of step (1) scale is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and tetraethoxy is 2.5: 1, and carry out the stirring of strong magnetic power, progressively instill distilled water, the mol ratio of distilled water and tetraethoxy is 1: 1, regulate its pH value to 4 ~ 5 with concentrated nitric acid, be hydrolyzed under room temperature reaction 2 hours, makes solution C;
(5), solution A, B and C are slowly mixed, after abundant mix and blend, then drip a certain amount of distilled water, the mol ratio of distilled water and tetraethoxy, aluminium secondary butylate, tri-n-butyl borate three summation is 0.5: 1, mixed hydrolysis makes solution D after reacting 0.5 hour;
(6), in solution D, add the measured strontium iodide of scale and the sub-europium of iodate in step (1), under vigorous stirring, hydrolysis reaction, after 2 hours, makes solution E;
(7), by after solution E sealing leave standstill 1 day, obtain the solution F of certain viscosity;
The preparation of film:
(8), solution F 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:
(9), the film that step (8) 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 high temperature hydrogen iodide Crystallizing treatment of film:
(10), the film that step (9) 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 50-60 per hour DEG C, progressively intensification stove is to 400-420 DEG C, and reaction treatment 2-5 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 divalent europium doping strontium iodide crystallite.
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, can effectively prevent divalent europium from changing into trivalent europium ion.
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 strontium 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 divalent europium and the strontium ion ion of glass network modifier, most one is in together in micropore gap, therefore along with the carrying out of high temperature hydrogen iodide process, divalent europium light emitting ionic easily enters in the lattice position of strontium iodide, obtains the rare earth ion doped and illumination effect of high density.
5, the hydrogen iodide drying treatment of high temperature impels iodine strontium oxide, strontium hydroxide and strontium oxide etc. in gel glass to convert strontium iodide to, can carry out the dehydration reaction of iodide raw material, and effectively promotes and the generation controlling strontium iodide crystallite.
Because this film glass matrix is SiO
2-Al
2o
3-B
2o
3three-phase system, therefore 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 divalent europium doping strontium iodide microcrystal silicon aluminum borate glass material, there is superior scintillation properties, physical strength, thermal stability characteristics, the shortcoming such as overcome strontium 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 the rare earth ion doped strontium iodide crystalline phase of divalent europium, obtained divalent europium doping strontium iodide devitrified glass film presents high transparency, 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 the thermal treatment of embodiment one high temperature hydrogen iodide;
Fig. 2 be embodiment one excitation of X-rays containing Eu
2+the fluorescence spectrum of the glass film of ion doping strontium 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 divalent europium doping strontium iodide crystallite, comprise the steps:
(1), rare earths material is pressed mole percentage composition: tetraethoxy: 74mol%, aluminium secondary butylate: 8mol%, tri-n-butyl borate: 7mol%, strontium iodide: 10mol%, sub-europium: the 1mol% of iodate, take analytically pure each raw materials that total amount is 20 grams, stand-by;
(2), the hydrolysis of aluminium secondary butylate: the aluminium secondary butylate of weighing in step (1) is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and aluminium secondary butylate is 3: 1, add Glacial acetic acid fast, the volume ratio of aluminium secondary butylate and Glacial acetic acid is 1: 1, and carry out the stirring of strong magnetic power, progressively instill distilled water, the mol ratio of distilled water and aluminium secondary butylate is 1: 1, be hydrolyzed under room temperature reaction 1 hour, makes solution A;
(3), the hydrolysis of tri-n-butyl borate: the tri-n-butyl borate of weighing in step (1) is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and tri-n-butyl borate is 2.5: 1, add Glacial acetic acid fast, the volume ratio of tri-n-butyl borate and Glacial acetic acid is 1: 1, and carry out the stirring of strong magnetic power, progressively instill distilled water, the mol ratio of distilled water and tri-n-butyl borate is 0.8: 1, be hydrolyzed under room temperature reaction 1 hour, makes solution B;
(4), the hydrolysis of tetraethoxy: the measured tetraethoxy of step (1) scale is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and tetraethoxy is 2.5: 1, and carry out the stirring of strong magnetic power, progressively instill distilled water, the mol ratio of distilled water and tetraethoxy is 1: 1, regulate its pH value to 4 ~ 5 with concentrated nitric acid, be hydrolyzed under room temperature reaction 2 hours, makes solution C;
(5), solution A, B and C are slowly mixed, after abundant mix and blend, then drip a certain amount of distilled water, the mol ratio of distilled water and tetraethoxy, aluminium secondary butylate, tri-n-butyl borate three summation is 0.5: 1, mixed hydrolysis makes solution D after reacting 0.5 hour;
(6), in solution D, add the measured strontium iodide of scale and the sub-europium of iodate in step (1), under vigorous stirring, hydrolysis reaction, after 2 hours, makes solution E;
(7), by after solution E sealing leave standstill 1 day, obtain the solution F of certain viscosity;
(8), solution F dip-coating method (dip-coating) is coated on clean glass substrate, the pull rate of glass substrate in gelating soln controls in 0.2 mm/second, lift can be repeated 1 time according to concrete thickness requirement, each lift interval time is 15 minutes, and the film after coating at room temperature dries 4 hours;
(9), the film that step (8) 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;
(10), the film that step (9) 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 400 DEG C, and reaction treatment 5 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 the SiO containing divalent europium doping strontium iodide crystallite
2-Al
2o
3-B
2o
3system glass film.
Performance test is carried out to the glass film containing divalent europium doping strontium iodide crystallite of preparation, 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 strontium iodide crystalline phase through processing the XRD diffraction peak of sample obtained, and what therefore obtain is the glass film containing strontium iodide crystallite.And the fluorescence spectrum of the divalent europium doping strontium iodide devitrified glass film of excitation of X-rays as shown in Figure 2, with the sample ratio without Crystallizing treatment, fluorescence intensity significantly strengthens.
Embodiment two
Substantially identical with embodiment one, difference be in step (1) by raw materials by following molar percentage: tetraethoxy: 65mol%, aluminium secondary butylate: 10mol%, tri-n-butyl borate: 10mol%, strontium iodide: 13mol%, sub-europium: the 2mol% of iodate, take each raw material respectively; In step (8), 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 (9), 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 (10), with the speed of 60 DEG C per hour, progressively intensification stove is to 420 DEG C, and reaction treatment 2 hours at such a temperature.
Carry out performance test to the glass film containing divalent europium doping strontium iodide crystallite prepared, 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 strontium iodide crystallite.The fluorescence spectrum of the glass film of the divalent europium doping strontium iodide crystallite of excitation of X-rays is substantially identical with Fig. 2, and compared with the sample without Crystallizing treatment, its fluorescence intensity significantly strengthens.
Embodiment three
Substantially identical with embodiment one, difference be in step (1) in by raw materials by following molar percentage: tetraethoxy: 70mol%, aluminium secondary butylate: 5mol%, tri-n-butyl borate: 5mol%, strontium iodide: 16mol%, sub-europium: the 4mol% of iodate, take each raw material respectively; In step (8), 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 (9), 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), with the speed of 55 DEG C per hour, progressively intensification stove is to 410 DEG C, and reaction treatment 3 hours at such a temperature.
Carry out performance test to the glass film containing divalent europium doping strontium iodide crystallite prepared, 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 strontium iodide crystallite.The fluorescence spectrum of the glass film of the divalent europium doping strontium iodide crystallite of excitation of X-rays is substantially identical with Fig. 2, and compared with the sample without Crystallizing treatment, its fluorescence intensity significantly strengthens.
Claims (1)
1., containing the preparation method of the glass film of divalent europium doping strontium iodide crystallite, it is characterized in that comprising the steps:
(1), raw materials is pressed mole percentage composition: tetraethoxy: 65-74mol%, aluminium secondary butylate: 5-10mol%, tri-n-butyl borate: 5-10mol%, strontium iodide: 10-16mol%, sub-europium: the 1-4mol% of iodate, take analytically pure each raw materials respectively, stand-by;
(2), the hydrolysis of aluminium secondary butylate: the aluminium secondary butylate of weighing in step (1) is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and aluminium secondary butylate is 3: 1, add Glacial acetic acid fast, the volume ratio of aluminium secondary butylate and Glacial acetic acid is 1: 1, and carry out the stirring of strong magnetic power, progressively instill distilled water, the mol ratio of distilled water and aluminium secondary butylate is 1: 1, be hydrolyzed under room temperature reaction 1 hour, makes solution A;
(3), the hydrolysis of tri-n-butyl borate: the tri-n-butyl borate of weighing in step (1) is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and tri-n-butyl borate is 2.5: 1, add Glacial acetic acid fast, the volume ratio of tri-n-butyl borate and Glacial acetic acid is 1: 1, and carry out the stirring of strong magnetic power, progressively instill distilled water, the mol ratio of distilled water and tri-n-butyl borate is 0.8: 1, be hydrolyzed under room temperature reaction 1 hour, makes solution B;
(4), the hydrolysis of tetraethoxy: the measured tetraethoxy of step (1) scale is dissolved in dehydrated alcohol, the mol ratio of dehydrated alcohol and tetraethoxy is 2.5: 1, and carry out the stirring of strong magnetic power, progressively instill distilled water, the mol ratio of distilled water and tetraethoxy is 1: 1, regulate its pH value to 4-5 with concentrated nitric acid, be hydrolyzed under room temperature reaction 2 hours, makes solution C;
(5), solution A, B and C are slowly mixed, after abundant mix and blend, then drip a certain amount of distilled water, the mol ratio of distilled water and tetraethoxy, aluminium secondary butylate, tri-n-butyl borate three summation is 0.5: 1, mixed hydrolysis makes solution D after reacting 0.5 hour;
(6), in solution D, add the measured strontium iodide of scale and the sub-europium of iodate in step (1), under vigorous stirring, hydrolysis reaction, after 2 hours, makes solution E;
(7), by after solution E sealing leave standstill 1 day, obtain the solution F of certain viscosity;
(8), solution F dip-coating method is coated on clean glass substrate, the pull rate of glass substrate in solution F 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;
(9), the film that step (8) 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;
(10), the film that step (9) 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 50-60 per hour DEG C, progressively intensification stove is to 400-420 DEG C, and reaction treatment 2-5 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 divalent europium doping strontium iodide crystallite.
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