CN105778901B - Eu2+Activate high-pure anhydrous halide of alkaline-earth metal and preparation method thereof - Google Patents
Eu2+Activate high-pure anhydrous halide of alkaline-earth metal and preparation method thereof Download PDFInfo
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Abstract
Eu is prepared the present invention relates to a kind of2+The method for activating the high-pure anhydrous halide of alkaline-earth metal, including mixed solution, concentration, dehydration and heat treatment step are prepared, it is M to obtain general formula1‑aEuaX2Target anhydrous halide, wherein M is one or both of alkali earth metal Mg, Ca, Sr, Ba, and X is one kind in halogens Cl, Br, I, 0.001<a≤0.2.Halide prepared by this method is free of the crystallization water and oxide impurity, has very high purity and good uniformity, can meet application demand of the materials such as scintillation crystal, scintillating ceramic to above-mentioned anhydrous halide.
Description
Technical field
The present invention relates to inorganic scintillation material fields；Eu is prepared in particular to a kind of2+Activate the high-purity nothing of alkaline-earth metal
Water halide and preparation method thereof.
Background technology
Scintillation material is a kind of material that optical photon can be sent out after absorbing the energy of high-energy ray or particle.It can
For the detection of the high energy particles such as the high-energy rays such as alpha ray, gamma-rays, X-ray and neutron, and nuclear medicine, high-energy physics,
Safety inspection, industrial non-destructive flaw detection, space physics and core mine locating etc. extensive application.They are usually with the shape of monocrystal
Formula is applied, and can also be glass, ceramics or other forms in some circumstances.
Eu2+Alkaline-earth halide scintillation material (such as SrI of activation2:Eu2+) light output because of its superelevation and splendid energy
Measure resolution ratio and by people's extensive concern, before the fields such as safety inspection, oil well logging, medical imaging have a wide range of applications
Scape.These scintillation materials are usually with high-pure anhydrous alkaline-earth halide and EuI2Crystal growth or preparation are carried out for raw material, but
Since these raw materials are all easily deliquesced and aoxidized, preparation is very difficult, therefore cost is very expensive, and existing market price is up to
Millions of dollars per kilogram seriously hinders the development and application of these scintillation materials.
Existing high-pure anhydrous alkaline-earth halide and EuI2Preparation method, typically with high-purity alkaline-earth metal and Eu
For raw material, with I2The direct chemical combination of simple substance obtains (metal iodide method).High-purity alkaline-earth metal and Eu are not only expensive, Er Qieji
It is active, it is easy to the alkaline earth metal iodide and EuI for aoxidizing, therefore being prepared using the method2Often contain more oxidation
Object impurity seriously affects the scintillation properties of material.Commercially available alkaline earth metal iodide and EuI2It need to could be used for after zone-refine
The growth of scintillation crystal, this causes production cost high.Therefore, a kind of efficiently high-pure anhydrous halogenation of low cost is found
Object preparation method, to Eu2+The development and application of the alkaline-earth halide scintillation material of activation are most important.
Chinese patent CN1651548A, which is disclosed, a kind of preparing Eu2+The side of the alkaline-earth halide scintillation material of activation
Method, this method use LiI and EuF3、Eu2O3, EuOF or Eu (OH)3The vacuum dehydration in quartz ampoule, then passes through Bridgman
Method grows crystal.However, the crystallization water and oxide impurity of the crystal that this method obtains are still unsatisfactory.Chinese patent
CN103818942A discloses a kind of method preparing high-pure anhydrous strontium iodide, and this method is that will to contain strontium compound anti-with hydroiodic acid
It answers, crystallization purifying after concentration, then vacuum dehydration.However, high-pure anhydrous strontium iodide has only been prepared in this method, do not obtain
Eu2+The high-pure anhydrous strontium iodide of activation；In addition, water and oxygen content are up to 1000ppm, purity is still to be improved.
Invention content
The purpose of the present invention is to provide a kind of simple and effective and low-cost Eu2+Activate alkaline-earth metal high-pure anhydrous
The preparation method of halide.
In order to achieve the above object, the present invention is quasi- uses following technical scheme：It is a kind of to prepare Eu2+Activate alkaline-earth metal high-purity
The method of anhydrous halide, including mixed solution, concentration, dehydration and heat treatment step are prepared, it is M to finally obtain general formula1-aEuaX2
Target anhydrous halide, wherein M is one or both of alkali earth metal Mg, Ca, Sr, Ba, X be halogens Cl,
One kind in Br, I, 0.001<a≤0.2；It is characterized in that：The dehydration be by alkaline-earth halide, europium halide and
The hybrid solid of ammonium halide carries out vacuum dehydration.The anhydrous halide prepared using this method is miscellaneous without the crystallization water and oxide
Matter has very high purity and good uniformity, can meet the materials such as scintillation crystal, scintillating ceramic to above-mentioned anhydrous halide
Application demand.
More specifically, preparation in accordance with the present invention includes the following steps：
(1) mixed solution of alkaline-earth halide, europium halide and ammonium halide is prepared；
(2) mixed solution is concentrated, the hybrid solid of alkaline-earth halide, europium halide and ammonium halide is obtained after cooling；
(3) hybrid solid of alkaline-earth halide, europium halide and ammonium halide is subjected to vacuum dehydration；
(4) material after dehydration is heat-treated, it is M to obtain general formula1-aEuaX2Target anhydrous halide.
Further, step (1) is：By the MCO of purity >=99.9%3、Eu2O3And NH4X is according to molar ratio (1-a):a/
2:(2~8) weighing, is dissolved in HX acid, obtains the clarification mixed solution of alkaline-earth halide, europium halide and ammonium halide.
Further, step (2) is：Mixed solution is concentrated into pulp dope at a temperature of 80~150 DEG C, then certainly
It is so cooled to room temperature, obtains the hybrid solid of alkaline-earth halide, europium halide and ammonium halide.
Further, step (3) is：The hybrid solid of alkaline-earth halide, europium halide and ammonium halide is placed in quartz
It in container, connects vacuum plant and heating device is dehydrated it, heating temperature is permanent after being to slowly warm up to 200~250 DEG C by room temperature
Temperature 2~48h, 2~30 DEG C/h of heating rate maintain quartz container vacuum degree≤3000Pa in dehydration.
Further, step (4) is：Material after dehydration is heat-treated, 400~600 DEG C of heating temperature, heating time
For 2~it is continually fed into high-purity dry Ar gas or N for 24 hours, in heating process2Gas shielded, in quartz container resultant product, that is, target without
Water halide.
On the other hand, the present invention relates to a kind of Eu2+Activate the high-pure anhydrous halide of alkaline-earth metal, which is characterized in that it is logical
Foregoing preparation method is crossed to obtain.It is preferred that purity >=99.9% of high-pure anhydrous halide, water content≤20ppm, oxygen contain
Amount≤100ppm.
Another aspect, the present invention relates to a kind of scintillation crystal, ceramics being prepared by aforementioned high-pure anhydrous halide
Or thin-film material.
It below will be with SrI2:Eu2+For the preparation of crystal, the technical characteristic of the present invention is illustrated.
SrI2:Eu2+The growth of crystal is usually with high-pure anhydrous SrI2、EuI2For raw material, the two is mixed according to a certain percentage
Afterwards, Vacuum Package is grown in silica crucible using Bridgman-Stockbarger method.With NH4I is dehydrating agent, to SrI2Hydrate into
Row vacuum dehydration can prepare the anhydrous SrI of very high-purity2.Inventor studies the reaction mechanism of the method, it is believed that
Its principle prepares anhydrous MgCl with " ammonium carnallite method "2It is similar, i.e. NH4I and SrI2There is certain coordination network during the dehydration process
Cooperation is used, to make SrI2Hydrolysis be inhibited.This method is equally applicable to anhydrous EuI2Preparation, but test find,
The EuI prepared using the method2Product contains more EuOI impurity.This is mainly due to EuI2With NH4The mating reaction of I is weaker,
Part EuI in dehydration2Caused by hydrolysis oxidation, therefore this method is difficult to obtain the anhydrous EuI of high-purity2Product.If with
NH4I is that dehydrating agent prepares SrI respectively2、EuI2The crystal growth raw material for mixing gained in proportion again afterwards, can be because of EuI2In containing compared with
More oxide impurity and cause whole purity insufficient.
For this problem, the present invention proposes, by SrI2And EuI2Mixed dehydration in proportion utilizes SrI2As main body
Matrix effect and SrI2、EuI2Between solid solution effect, to inhibit EuI2Hydrolysis oxidation tendency in dehydration.Experimental result
Show that this method has good actual effect.Work as EuI2When molar content is less than 20%, SrI2Matrix effect it is fairly obvious,
Products obtained therefrom oxygen content is very low, is substantially free of iodine oxidation europium impurity；Work as EuI2When molar content is higher than 20%, SrI2Matrix effect
It should be with EuI2The increase of content and gradually weaken, product oxygen content gradually rises, and illustrates containing more iodine oxidation europium impurity.By
The SrI in open source literature2:The molar fraction of Eu is typically not greater than 20% in Eu scintillation materials, therefore the present invention can expire completely
Sufficient SrI2:The component requirements of Eu scintillation materials.This method is extended to other Eu2+The system of adulterated alkaline-earth metal anhydrous halide
It is standby, find that equally there is good effect.
Another benefit in fact can also be provided in the present invention, that is, improves activator ion Eu2+It is uniform in scintillation material
Property.Anhydrous halide produced by the present invention is that chemical formula is M1-aEuaX2Homogeneous solid solution, compare MX2、EuX2Later stage it is mixed
It closes, Eu2+Ion is more uniformly spread, this is of great advantage for the homogeneity for improving scintillation material.
Dehydrating agent NH in the present invention4The use of X is for obtaining the particularly significant without aquatic products of high-purity.Experimental result table
Bright, when dosage is 2 to 8 times (mole) of metal iodide, effect is ideal.Very few NH4X dosages do not have inhibition
The effect of hydrolysis, and excessive NH4X dosages are not only not necessarily to, but also can cause the decline of yield.
It (is prepared as the direct combination reaction of raw material using high pure metal and high-purity halogen simple substance compared to common metal halide method
Anhydrous metal halide), raw material used in the present invention is alkaline earth metal carbonate, europium oxide, halogen acids and ammonium halide, is compared
High pure metal and high-purity halogen, cost will inexpensively much be also easier to produce in enormous quantities, therefore be answered with preferably industrialization
Use foreground.Relative to first dehydration prepares anhydrous MI respectively2And EuI2, again in proportion mixing obtain M1-aEuaX2The method of material,
Present invention process is more simple, and products obtained therefrom purity higher, especially oxide impurity content is relatively low, and activator distribution is more
Uniformly, the demand more suitable for materials such as scintillation crystal, ceramics to raw material.
Specific implementation mode
It is illustrated with reference to specific embodiment.
Comparative example 1：Accurately weigh 147.6g SrCO3(99.95%), 738g NH4I (99.9%) is dissolved in hydroiodic acid and obtaining
To mixing clear solution, it is in starchiness that 100 DEG C, which are concentrated into material, and blocky drying solid is obtained after natural cooling.By blocks of solid
It is contained in quartzy dehydrating tube after broken, is put into tube furnace and is dehydrated.Dehydration temperaturre is to slowly warm up to 250 DEG C by room temperature and is kept the temperature
15h, 15 DEG C/h of heating rate, is during which vacuumized using water ring pump, vacuum degree about 2100Pa.It is high-purity then to being filled in quartz ampoule
Dry Ar gas, and 500 DEG C are warming up to, constant temperature 2h obtains anhydrous SrI after cooling2Product.It is 18ppm, oxygen to detect its water content
Content is 49ppm.Separately weigh 17.6g Eu2O3(99.99%), 43.5g NH4I (99.9%) is dissolved in obtaining in hydroiodic acid
To clear solution, it is in starchiness that 100 DEG C, which are concentrated into material, and blocky drying solid is obtained after natural cooling.Fast-turn construction solid is crushed
After be contained in quartzy dehydrating tube, be put into tube furnace and be dehydrated.Dehydration temperaturre is to slowly warm up to 220 DEG C by room temperature and keeps the temperature 15h, rises
15 DEG C/h of warm rate, is during which vacuumized using water ring pump, vacuum degree about 2300Pa.Then to being filled with high-purity dry Ar in quartz ampoule
Gas, and 450 DEG C are warming up to, constant temperature 5h obtains anhydrous EuI2Product.It is 21ppm, oxygen content about 2400ppm to detect its water content.
Weigh 162.2 g SrI2With 10.1g EuI2, 560 DEG C are heated under Ar gas shieldeds after mixing and is allowed to melt, after cooling
Obtaining group becomes Sr0.95Eu0.05I2Blocky anhydrous halide.It is 12ppm, oxygen content 236ppm to detect its water content.
Embodiment 1：Accurately weigh 140.2g SrCO3(99.95%), 8.8g Eu2O3(99.99%), 434.9 g NH4I
(99.9%), it is dissolved in hydroiodic acid and obtains mixing clear solution, it is in starchiness that 110 DEG C, which are concentrated into material, is obtained after natural cooling
Blocky drying solid.It is contained in quartzy dehydrating tube after blocks of solid is crushed, is put into tube furnace and is dehydrated.Dehydration temperaturre is by room temperature
It is to slowly warm up to 250 DEG C and keeps the temperature 2h, during which 2 DEG C/h of heating rate is vacuumized using water ring pump, vacuum degree about 2100Pa.With
It is filled with high-purity dry Ar gas in backward quartz ampoule, and is warming up to 400 DEG C, constant temperature 2h, obtaining group after cooling becomes
Sr0.95Eu0.05I2Anhydrous halide product.It is 11ppm, oxygen content 47ppm to detect its water content.
Embodiment 2：Accurately weigh 195.4g BaCO3(99.95%), 1.8g Eu2O3(99.99%), 391.8 g
NH4Br (99.9%) is dissolved in hydrobromic acid and obtains mixing clear solution, and it is in starchiness that 80 DEG C, which are concentrated into material, after natural cooling
Obtain blocky drying solid.It is contained in quartzy dehydrating tube after blocks of solid is crushed, is put into tube furnace and is dehydrated.Dehydration temperaturre by
Room temperature is to slowly warm up to 200 DEG C and keeps the temperature 48h, and during which 10 DEG C/h of heating rate is vacuumized using water ring pump, vacuum degree is about
2400Pa.Then to being filled with high-purity dry Ar gas in quartz ampoule, and 600 DEG C are warming up to, constant temperature 2h, obtaining group after cooling becomes
Ba0.99Eu0.01Br2Anhydrous halide product.It is 8ppm, oxygen content 41ppm to detect its water content.
Embodiment 3：Accurately weigh 90.1g CaCO3(99.95%), 17.6g Eu2O3(99.99%), 160.5 g
NH4Cl (99.9%) is dissolved in hydrochloric acid and obtains mixing clear solution, and it is in starchiness that 120 DEG C, which are concentrated into material, after natural cooling
To blocky drying solid.It is contained in quartzy dehydrating tube after blocks of solid is crushed, is put into tube furnace and is dehydrated.Dehydration temperaturre is by room
Temperature is to slowly warm up to 250 DEG C and keeps the temperature for 24 hours, and during which 8 DEG C/h of heating rate is vacuumized using water ring pump, vacuum degree about 2300Pa.
Then to being filled with high-purity dry Ar gas in quartz ampoule, and 580 DEG C are warming up to, constant temperature 4h, obtaining group after cooling becomes
Ca0.9Eu0.1Cl2Anhydrous halide product.It is 12ppm, oxygen content 58ppm to detect its water content.
Embodiment 4：Accurately weigh 82.6g MgCO3(99.95%), 3.5g Eu2O3(99.99%), 214.0 g NH4Cl
(99.9%), it is dissolved in hydroiodic acid and obtains mixing clear solution, it is in starchiness that 150 DEG C, which are concentrated into material, is obtained after natural cooling
Blocky drying solid.It is contained in quartzy dehydrating tube after blocks of solid is crushed, is put into tube furnace and is dehydrated.Dehydration temperaturre is by room temperature
It is to slowly warm up to 220 DEG C and keeps the temperature 8h, during which 15 DEG C/h of heating rate is vacuumized using water ring pump, vacuum degree about 2400Pa.
Then to being filled with high-purity dry Ar gas in quartz ampoule, and 500 DEG C are warming up to, constant temperature 12h, obtaining group after cooling becomes
Mg0.98Eu0.02I2Anhydrous halide product.It is 8ppm, oxygen content 39ppm to detect its water content.
Embodiment 5：Accurately weigh 59.2g BaCO3(99.95%), 8.4g MgCO3(99.95%), 17.6g Eu2O3
(99.99%), 362.3g NH4I (99.9%) is dissolved in hydroiodic acid and obtains mixing clear solution, and 130 DEG C are concentrated into material and are in
Starchiness obtains blocky drying solid after natural cooling.It is contained in quartzy dehydrating tube after blocks of solid is crushed, is put into tube furnace
Middle dehydration.Dehydration temperaturre is to slowly warm up to 250 DEG C by room temperature and keeps the temperature 20h, 20 DEG C/h of heating rate, during which uses water ring pump
It vacuumizes, vacuum degree about 2200Pa.Then to being filled with high-purity dry N in quartz ampoule2Gas, and be warming up to 540 DEG C, constant temperature 3h are cold
But obtaining group afterwards becomes Ba0.6Mg0.2Eu0.2I2Anhydrous halide product.It is 13ppm to detect its water content, and oxygen content is
52ppm。
Embodiment 6：Accurately weigh 125.5g SrCO3(99.95%), 26.4g Eu2O3(99.99%), 293.9g
NH4Br (99.9%) is dissolved in hydrobromic acid and obtains mixing clear solution, and it is in starchiness that 90 DEG C, which are concentrated into material, after natural cooling
Obtain blocky drying solid.It is contained in quartzy dehydrating tube after blocks of solid is crushed, is put into tube furnace and is dehydrated.Dehydration temperaturre by
Room temperature is to slowly warm up to 250 DEG C and keeps the temperature 10h, and during which 30 DEG C/h of heating rate is vacuumized using water ring pump, vacuum degree is about
2100Pa.Then to being filled with high-purity dry N in quartz ampoule2Gas, and 450 DEG C are warming up to, constant temperature 20h, obtaining group after cooling becomes
Sr0.85Eu0.15Br2Anhydrous halide product.It is 7ppm, oxygen content 33ppm to detect its water content.
By comparing it can be found that the high-pure anhydrous halide water content that the preparation method of 1-6 of the embodiment of the present invention obtains
Very low, minimum is only 7 ppm；Minimum only 33 ppm of oxygen content, wherein water content are suitable or more excellent with 1 result of comparative example；
Oxygen content is substantially less than comparative example 1.The above results show that high-pure anhydrous halide of the invention is miscellaneous without the crystallization water and oxide
Matter has very high purity and good uniformity, can meet the materials such as scintillation crystal, scintillating ceramic to above-mentioned anhydrous halide
Application demand.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of preparing Eu2+The method for activating the high-pure anhydrous halide of alkaline-earth metal, including prepare mixed solution, concentration, dehydration
And heat treatment step, it is M to finally obtain general formula1-aEuaX2Target anhydrous halide, wherein M be alkali earth metal Mg, Ca,
One or both of Sr, Ba, X are one kind in halogens Cl, Br, I, 0.001 a≤0.2 <；It is characterized in that：It is described
Dehydration is that the hybrid solid of alkaline-earth halide, europium halide and ammonium halide is carried out vacuum dehydration.
2. preparation method according to claim 1, the method includes the steps of：
(1) mixed solution of alkaline-earth halide, europium halide and ammonium halide is prepared；
(2) mixed solution is concentrated, the hybrid solid of alkaline-earth halide, europium halide and ammonium halide is obtained after cooling；
(3) hybrid solid of alkaline-earth halide, europium halide and ammonium halide is subjected to vacuum dehydration；
(4) material after dehydration is heat-treated, it is M to obtain general formula1-aEuaX2Target anhydrous halide.
3. preparation method according to claim 2, wherein the step (1) is：By the MCO of purity >=99.9%3、Eu2O3
And NH4X is according to molar ratio (1-a):a/2:(2~8) weighing, is dissolved in HX acid, obtains alkaline-earth halide, europium halide and halogen
Change the clarification mixed solution of ammonium.
4. preparation method according to claim 2, wherein the step (2) is：By mixed solution in 80~150 DEG C of temperature
Lower concentration pulp dope, subsequent cooled to room temperature obtain the mixing of alkaline-earth halide, europium halide and ammonium halide
Solid.
5. preparation method according to claim 2, wherein the step (3) is：By alkaline-earth halide, europium halide and
The hybrid solid of ammonium halide is placed in quartz container, connects vacuum plant and heating device is dehydrated it, heating temperature is by room temperature
2~48h of constant temperature after being to slowly warm up to 200~250 DEG C, 2~30 DEG C/h of heating rate maintain quartz container vacuum in dehydration
Degree≤3000Pa.
6. preparation method according to claim 2, wherein the step (4) is：Material after dehydration is heat-treated, is added
400~600 DEG C of hot temperature, heating time be 2~be continually fed into high-purity dry Ar gas or N for 24 hours, in heating process2Gas shielded, stone
Resultant product, that is, target anhydrous halide in English container.
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