CN106542813A - The method for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder - Google Patents
The method for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder Download PDFInfo
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Abstract
The invention discloses one kind is directly with nano silicon as raw material, urea is auxiliary precipitating reagent, the method for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder.Luteium oxide powder is dissolved with concentrated hydrochloric acid and prepares lutetium ion solution, obtained solution is mixed with urea, nano silicon, product presoma is obtained after heating response, precipitation, centrifugation, dried presoma are calcined by Muffle furnace high temperature, described nanoscale lutetium silicate polycrystal scintillating ceramic powder is obtained.Needed for presoma obtained in this method, calcining heat is low, nano silicone acid lutetium polycrystalline scintillating ceramic powder is obtained after calcining, powder granule is in corynebacterium, grain diameter is 200 300nm, compared to traditional preparation methods such as direct precipitation method, sol-gal processes, its cost is lower, preparation technology is simpler, it is easier to realize batch, industrialized production manufacture.
Description
Technical field
The present invention relates to scintillating ceramic Preparation Technique of Powders field, more particularly to one kind prepares the sudden strain of a muscle of nanoscale lutetium silicate polycrystal
The method of bright ceramic powder.
Background technology
Silicic acid lutetium Lu2SiO5(LSO) with excellent scintillation properties, it is the inorganic scintillation material of current most competitiveness.Silicon
Sour lutetium scintillation crystal is a kind of scintillation material of excellent combination property, and which has high density, High Light Output, high light yield, decay
Time is short, it is adaptable to the field such as medical imaging, space physics, high-energy physics, industrial flaw detection, geological prospecting.Ceramic scintillation materials
Although light output is not so good as crystal scintillation material, ceramic scintillation materials typically have the good transparency and stability, intensity is high,
Good insulating, being capable of high temperature resistant, corrosion-resistant.Ceramic scintillation materials production is time-consuming short, and to equipment requirement, high cost is not low so as to send out
Exhibition does not have the such many constraints of crystal scintillation material and limits with application.Ceramic scintillation materials are due to structure unlike crystalline material will
Ask regular like that, so it can preferably realize the Uniform Doped of variable concentrations exciting agent, this can be good at improving flicker
The luminescent properties of material.The purity of scintillating ceramic powder, dispersiveness, second phase uniform doping etc. are to affect ceramic post sintering performance
Key factor, and determine scintillating ceramic performance key issue.
Due to up to 2000 DEG C of silicic acid lutetium fusing point, using tradition lifting Laue method prepare lutecium silicate crystal material cost compared with
Height, prepare it is difficult, and rare earth ion in silicic acid lutetium matrix, segregation coefficient is little cannot realize Uniform Doped, compare with monocrystalline,
Polycrystalline ceramic possess relatively low cost, short preparation period, constituent structure such as can design at the advantage.Polycrystalline silicic acid lutetium scintillating ceramic powder
The preparation method of body mainly has solid phase mixing calcination method, the precipitation method and sol-gal process.Solid phase mixing calcination method prepares polysilicon
Sour lutetium powder, preparation process is simple, but reaction temperature are high, and the reaction time is long, and product is bulk, and be unfavorable for ceramic material enters one
Step prepares processing.Liquid-phase precipitation method prepares lutetium silicate polycrystal ceramic powder diameter of particle for tens microns, and phase purity is not high, holds
It is easily introduced impurity.Sol-gal process prepares lutetium silicate polycrystal ceramic powder and film, powder granule even size distribution, particle
Size about 400-500nm, but experimentation complex operation, yield poorly, are not suitable for mass production.Silicic acid lutetium LSO and some
Common crystal scintillation material scintillation properties contrast sees attached list 1.
Some the conventional scintillator crystal materials of table 1 are contrasted with LSO scintillation properties
The content of the invention
It is an object of the invention to provide a kind of method for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder.Obtained
Calcining heat needed for precursor product is low, particle be in corynebacterium, grain diameter is 200-300nm, compared to direct precipitation method,
The traditional preparation methods such as sol-gal process are easier, and production cost is lower, and preparation method is simpler, it is easier to realization batch,
Industrialized production is manufactured.
To achieve these goals, the technical scheme is that：One kind prepares nanoscale lutetium silicate polycrystal scintillating ceramic
The method of powder, it is characterised in that methods described comprises the steps：
1) with nano silicon as silicon source, addition urea is as aids precipitation agent, anti-with lutecium chloride solution Hybrid Heating
White presoma emulsion should be generated；
2) white presoma emulsion staticly settled, centrifugation, obtain a nanometer silicic acid lutetium powder presoma after drying
Product；
3) nanometer silicic acid lutetium powder precursor product is carried out after high-temperature calcination by Muffle furnace, particle diameter is obtained for 200-
The nanoscale lutetium silicate polycrystal scintillating ceramic powder of 300nm.
Further, the described method for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder, it is characterised in that step
1) the white presoma emulsion preparation process described in comprises the steps：
1.1) by luteium oxide Lu2O3Powder heating is dissolved in concentrated hydrochloric acid HCl, and concentrated hydrochloric acid is (6-10) with luteium oxide mol ratio:
1, obtain clarifying LuCl3Solution, adds a certain amount of deionized water dilution, makes lutetium ion Lu in solution3+Concentration is 0.5-0.8mol/
L；
1.2) by urea and lutetium ion Lu3+Molar ratio is (30-120):1 urea for weighing certain mass adds step
1.1) 2h-4h is stirred in the solution for obtaining, obtain lutetium ion Lu3+With the mixed solution of urea；
1.3) Lu in molar ratio:Si=2:1 weighs certain mass nano silica powder is dissolved in deionized water, ultrasound point
Scattered 10-15min, obtains nanosilica solution；
1.4) by step 1.3) nanosilica solution that obtains adds step 1.2) the lutetium ion Lu that obtains3+With urea
Mixed solution in, mix, heating response 4-6h, obtain described white presoma emulsion.
Further, the described method for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder, it is characterised in that step
2) its actual conditions that is dried described in is：24-48h is dried under the conditions of 85-95 DEG C in an oven.
Further, the described method for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder, it is characterised in that step
3) the calcining heat mechanism of the nanometer silicic acid lutetium powder precursor product described in is：
In air atmosphere, the calcining of Muffle furnace high temperature, rises to 400-500 DEG C with the heating rate of 5-10 DEG C/min, protects
Warm 1-2h；
900-1100 DEG C is warming up to the heating rate of 3-7 DEG C/min, 1-3h is incubated.
The invention has the beneficial effects as follows：The method for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder of the present invention, directly
Connect with nano silicon SiO2 as silicon source, nanometer silicic acid lutetium powder presoma, obtained nanometer silicic acid lutetium powder forerunner is obtained
Needed for body, calcining heat is low, and nano silicone acid lutetium polycrystalline scintillating ceramic powder is obtained after calcining, and powder granule is in corynebacterium,
Grain particle diameter is less for 200-300nm, and compared to traditional preparation methods such as direct precipitation method, sol-gal processes, its cost is lower, system
Standby technique is simpler, it is easier to realize batch, industrialized production manufacture.
Description of the drawings
Fig. 1 is shown by the method flow for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder that the embodiment of the present invention is provided
It is intended to；
Fig. 2 is the X ray diffracting spectrum and silicic acid lutetium standard phase PDF card of the scintillating ceramic powder described in the embodiment of the present invention
The comparison diagram of piece, both diffraction maximums are corresponded, and are the presence for finding impurity peaks, illustrate to dodge using silicic acid lutetium obtained in the present invention
Bright ceramic powder body phase purity is high, and free from admixture is mutually present.
Fig. 3 is the field emission scanning electron microscope figure of the scintillating ceramic powder described in the embodiment of the present invention.
Specific embodiment
With reference to embodiment and accompanying drawing, clear, complete description is carried out to the technical scheme in the embodiment of the present invention, shown
And be clear to, described embodiment a part of embodiment only of the invention, rather than whole embodiments.Based on the present invention's
Embodiment, the every other embodiment obtained under the premise of creative work is not made by those of ordinary skill in the art, all
Belong to protection scope of the present invention.
The method that nanoscale lutetium silicate polycrystal scintillating ceramic powder is prepared described in the embodiment of the present invention is to first pass through lutetium ion
Precursor product is obtained with urea, nanometer titanium dioxide pasc reaction, then precursor product passes through high-temperature calcination system in Muffle furnace
It is standby go out nanoscale silicic acid lutetium scintillating ceramic powder.The embodiment of the present invention is described in further detail below in conjunction with accompanying drawing, such as
The method flow schematic diagram for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder that Fig. 1 is provided by the embodiment of the present invention, institute
The method of stating includes：
Lutecium chloride solution is prepared with concentrated hydrochloric acid dissolving luteium oxide, then will be lutecium chloride solution anti-with urea, nano silicon
Presoma emulsion should be generated, emulsion is staticly settled, centrifugation, obtain precursor product after drying.
The concrete preparation process of precursor product described in the step is：
By luteium oxide Lu2O3Powder heating is dissolved in concentrated hydrochloric acid HCl, and concentrated hydrochloric acid is (6-10) with luteium oxide mol ratio:1, obtain
To clarification LuCl3Solution, adds deionized water dilution to make lutetium ion Lu in solution3+Concentration is 0.5-0.8mol/L；
It is (30-120) by urea and metal ion molar ratio:1 urea for weighing certain mass is stirred in adding solution
2-4h, obtains lutetium ion Lu3+With the mixed solution of urea；
Lu in molar ratio:Si=2:1 weighs certain mass nano silica powder is dissolved in deionized water, ultrasonic disperse
10-15min, obtains nanosilica solution；
The nano silicon for obtaining is added into lutetium ion Lu3+In the mixed solution of urea, agitating heating reaction 4-6h,
Obtain white presoma emulsion；
Presoma emulsion is staticly settled, centrifugation, obtain after being dried 24-48h under the conditions of 85-95 DEG C in an oven
Described nanometer silicic acid lutetium powder precursor product.
Precursor product prepares nanoscale lutetium silicate polycrystal scintillating ceramic powder by Muffle furnace high-temperature calcination.
The calcining heat mechanism of described nanometer silicic acid lutetium powder precursor product is：
In air atmosphere, the calcining of Muffle furnace high temperature, rises to 400-500 DEG C with the heating rate of 5-10 DEG C/min, protects
Warm 1-2h；
900-1100 DEG C is warming up to the heating rate of 3-7 DEG C/min, 2-3h is incubated.
The method for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder, directly with nano silicon SiO2For silicon
Source, is obtained precursor product.
Carry out checking explanation below to the performance of prepared nanoscale lutetium silicate polycrystal scintillating ceramic powder, Fig. 2 is front
Drive the X ray diffracting spectrum and standard phase PDF card of the silicic acid lutetium scintillating ceramic powder obtained after body is calcined at 1100 DEG C
Comparison diagram.As shown in Figure 2：Silicic acid lutetium crystalline phase needed for being successfully obtained using the preparation method described in the present embodiment, in collection of illustrative plates
It was found that impurities phase diffraction maximum, the silicic acid lutetium scintillating ceramic powder phase purity obtained by the present embodiment is very high, and free from admixture is mutually deposited
, needed for presoma, calcining heat is low, under the conditions of 1100 DEG C be it is crystallizable generation silicic acid lutetium scintillating ceramic powder.
Fig. 3 is to be sent out using the field under silicic acid lutetium ceramic powder different resolution obtained in the preparation method described in the present embodiment
Penetrate scanning electron microscope (SEM) photograph., in corynebacterium, grain diameter is less, is 200-300nm for powder granule as seen from the figure.
Above-mentioned preparation process is illustrated with specific example below：
Embodiment 1：
By concentrated hydrochloric acid and luteium oxide mol ratio 8:1, first by 5.2129 grams of Lu2O3, 10.00ml deionized waters heating be dissolved in
In 8.66ml concentrated hydrochloric acids, 43.00ml deionized waters after dissolving completely, are added to make lutetium ion Lu in solution3+Concentration is 0.6mol/L.
It is 30 by urea and metal ion ratio:1 weighs during 47.40566 grams of urea add solution and stirs 2h.
By Lu:Si=2:1 weighs 0.7903 gram of nano silica powder is dissolved in deionized water, ultrasonic disperse 15min.
Nano silicon is added into lutetium ion Lu3+In the mixed solution of urea, agitating heating reaction 5h obtains white
Presoma emulsion.
White presoma emulsion is stood, centrifugation, obtain a nanometer silicic acid after being dried 24h at being put into 90 DEG C in baking oven
Lutetium powder presoma.
By nanometer silicic acid lutetium powder presoma by Muffle furnace high-temperature calcination, first risen to the heating rate of 10 DEG C/min
400 DEG C, 1h is incubated, then 1000 DEG C is warming up to the heating rate of 5 DEG C/min, be incubated 2h, obtain final product the sudden strain of a muscle of nanoscale lutetium silicate polycrystal
Bright ceramic powder.
Embodiment 2：
By concentrated hydrochloric acid and luteium oxide mol ratio 10:1, first by 5.2320 grams of Lu2O3, 10.00ml deionized waters heating be dissolved in
In 10.83ml concentrated hydrochloric acids, 43.00ml deionized waters after dissolving completely, are added to make lutetium ion Lu in solution3+Concentration is 0.6mol/L.
It is 60 by urea and metal ion ratio:1 weighs during 94.8112 grams of urea add solution and stirs 2h.
By Lu:Si=2:1 weighs 0.7903 gram of nano silica powder is dissolved in deionized water, ultrasonic disperse 15min.
Nano silicon is added into lutetium ion Lu3+In the mixed solution of urea, agitating heating reaction 5h obtains white
Presoma emulsion.
White presoma emulsion is stood, centrifugation, obtain a nanometer silicic acid after being dried 24h at being put into 90 DEG C in baking oven
Lutetium powder presoma.
By nanometer silicic acid lutetium powder presoma by Muffle furnace high-temperature calcination, first risen to the heating rate of 10 DEG C/min
500 DEG C, 1h is incubated, then 1050 DEG C is warming up to the heating rate of 5 DEG C/min, be incubated 2h, obtain final product the sudden strain of a muscle of nanoscale lutetium silicate polycrystal
Bright ceramic powder.
Embodiment 3：
By concentrated hydrochloric acid and luteium oxide mol ratio 6:1, first by 5.2320 grams of Lu2O3, 10.00ml deionized waters heating be dissolved in
In 6.49ml concentrated hydrochloric acids, 43.00ml deionized waters after dissolving completely, are added to make lutetium ion Lu in solution3+Concentration is 0.6mol/L.
It is 90 by urea and metal ion ratio:1 weighs during 142.2168 grams of urea add solution and stirs 2h.
By Lu:Si=2:1 weighs 0.7903 gram of nano silica powder is dissolved in deionized water, ultrasonic disperse 15min.
Nano silicon is added into lutetium ion Lu3+In the mixed solution of urea, agitating heating reaction 4h obtains white
Presoma emulsion.
White presoma emulsion is stood, centrifugation, obtain a nanometer silicic acid after being dried 24h at being put into 90 DEG C in baking oven
Lutetium powder presoma.
By nanometer silicic acid lutetium powder presoma by Muffle furnace high-temperature calcination, first risen to the heating rate of 10 DEG C/min
450 DEG C, 1h is incubated, then 1100 DEG C is warming up to the heating rate of 5 DEG C/min, be incubated 2h, obtain final product the sudden strain of a muscle of nanoscale lutetium silicate polycrystal
Bright ceramic powder.
Embodiment 4：
By concentrated hydrochloric acid and luteium oxide mol ratio 8:1, first by 5.2320 grams of Lu2O3, 10.00ml deionized waters heating be dissolved in
In 9.00ml concentrated hydrochloric acids, 43.00ml deionized waters after dissolving completely, are added to make lutetium ion Lu in solution3+Concentration is 0.6mol/L.
It is 120 by urea and metal ion ratio:1 weighs during 189.6244 grams of urea add solution and stirs 2h.
By Lu:Si=2:1 weighs 0.7903 gram of nano silica powder is dissolved in deionized water, ultrasonic disperse 15min.
Nano silicon is added into lutetium ion Lu3+In the mixed solution of urea, agitating heating reaction 5h obtains white
Presoma emulsion.
White presoma emulsion is stood, centrifugation, obtain a nanometer silicic acid after being dried 24h at being put into 90 DEG C in baking oven
The presoma of lutetium powder.
By nanometer silicic acid lutetium powder presoma by Muffle furnace high-temperature calcination, first risen to the heating rate of 10 DEG C/min
500 DEG C, 1h is incubated, then 1100 DEG C is warming up to the heating rate of 5 DEG C/min, be incubated 2h, obtain final product the sudden strain of a muscle of nanoscale lutetium silicate polycrystal
Bright ceramic powder.
In sum, the preparation method and obtained product for adopting described in the present embodiment has advantages below：
1) directly with nano silicon as silicon source, cost of material is cheap, and old low, easy to operate；
2) powder granule particle diameter obtained by is less for 200-300nm, belongs to nanometer grade powder；
3) the phase purity of powder obtained by is high, does not find the presence of impurities phase；
4) traditional preparation methods such as contrast and solid reaction process, needed for presoma, sintering temperature is low, can knot at 1100 DEG C
It is brilliant to generate nanometer silicic acid lutetium scintillating ceramic powder.
The above, only summarizes the preferably embodiment of the present invention for obtaining, but the guarantor of the present invention after many experiments
Shield scope is not limited thereto, and any those skilled in the art, can be easily in presently disclosed technical scope
The change for obtaining or conversion, should all be included within the scope of the present invention.Therefore protection scope of the present invention should be with power
The protection domain of sharp claim is defined.
Claims (4)
1. a kind of method for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder, it is characterised in that methods described includes as follows
Step：
1) with nano silicon as silicon source, addition urea is given birth to the reaction of lutecium chloride solution Hybrid Heating as aids precipitation agent
Into white presoma emulsion；
2) white presoma emulsion staticly settled, centrifugation, obtain a nanometer silicic acid lutetium powder precursor product after drying；
3) nanometer silicic acid lutetium powder precursor product is carried out after high-temperature calcination by Muffle furnace, particle diameter is obtained for 200-300nm
Nanoscale lutetium silicate polycrystal scintillating ceramic powder.
2. the method for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder according to claim 1, it is characterised in that step
It is rapid 1) described in white presoma emulsion preparation process comprise the steps：
1.1) by luteium oxide Lu2O3Powder heating is dissolved in concentrated hydrochloric acid HCl, and concentrated hydrochloric acid is (6-10) with luteium oxide mol ratio:1, obtain
To clarification LuCl3Solution, adds a certain amount of deionized water dilution, makes lutetium ion Lu in solution3+Concentration is 0.5-0.8mol/L；
1.2) by urea and lutetium ion Lu3+Molar ratio is (30-120):1 urea for weighing certain mass adds step 1.1)
To solution in stir 2h-4h, obtain lutetium ion Lu3+With the mixed solution of urea；
1.3) Lu in molar ratio:Si=2:1 weighs certain mass nano silica powder is dissolved in deionized water, ultrasonic disperse
10-15min, obtains nanosilica solution；
1.4) by step 1.3) nanosilica solution that obtains adds step 1.2) the lutetium ion Lu that obtains3+It is mixed with urea
Close in solution, mix, heating response 4-6h, obtain described white presoma emulsion.
3. the method for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder according to claim 1 and 2, its feature exist
In step 2) described in its actual conditions that is dried be：24-48h is dried under the conditions of 85-95 DEG C in an oven.
4. the method for preparing nanoscale lutetium silicate polycrystal scintillating ceramic powder according to claim 1 and 2, its feature exist
In step 3) described in the calcining heat mechanism of nanometer silicic acid lutetium powder precursor product be：
In air atmosphere, the calcining of Muffle furnace high temperature, rises to 400-500 DEG C with the heating rate of 5-10 DEG C/min, is incubated 1-
2h；
900-1100 DEG C is warming up to the heating rate of 3-7 DEG C/min, 1-3h is incubated.
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| CN115028451A (en) * | 2022-06-28 | 2022-09-09 | 中国工程物理研究院化工材料研究所 | Preparation method of terbium oxide nano powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115028451A (en) * | 2022-06-28 | 2022-09-09 | 中国工程物理研究院化工材料研究所 | Preparation method of terbium oxide nano powder |
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