CN114988876B - Eu and Sc co-doped transparent lutetium oxide ceramic and preparation method thereof - Google Patents
Eu and Sc co-doped transparent lutetium oxide ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a Eu and Sc co-doped transparent lutetium oxide ceramic and a preparation method thereof, wherein the content of cations in the ceramic is calculated, and europium oxide and scandium oxide are calculated according to Eu 3+ The solid solution concentration is 1 to 8at percent, sc 3+ The solid solution concentration is 5 to 45at percent and is doped into lutetium oxide, lu 3+ The solid solution concentration is 49-91%. The doping step comprises the following steps in sequence: ball milling, molding, sintering and annealing the raw materials. Compared with the traditional Eu-doped lutetium oxide-based material system, the Eu-Sc co-doped transparent lutetium oxide ceramic prepared by the invention has the characteristics of short afterglow time, high luminous efficiency and high transmittance.
Description
Technical Field
The invention relates to the field of transparent ceramics, in particular to a novel scintillator material system for high-energy ray detection and a novel preparation method. More specifically, the present invention relates to a novel (Eu x Sc y Lu 1-x-y ) 2 O 3 Transparent scintillator ceramics and a method for preparing the same.
Background
Lutetium oxide (Lu) 2 O 3 ) Belongs to a cubic crystal system, has very high transmittance in the visible and near infrared bands, and has higher density reaching 9.42g/cm 3 Can effectively block X-rays and is applied to the field of high-energy X-ray detection. Doped with europium ions (Eu) 3+ ) The lutetium oxide can convert high-energy rays into visible light for emission, has narrow emission wavelength, can be well coupled with an industrial CCD detection sensitive range, and has wide application prospects in the fields of national security, medical examination, space detection and the like. However, the melting point of lutetium oxide materials is very high (exceeding 2400 ℃), and it is very difficult to grow crystals, and reliable techniques for obtaining large-size Eu-doped lutetium oxide single crystals are still lacking. The preparation of the lutetium oxide transparent ceramic does not need too high temperature, has the advantages of low cost, short preparation time and the like, and can be relatively compatibleThe preparation method is easy to realize large size and is an ideal preparation method of the lutetium oxide scintillation material.
The Eu-doped lutetium oxide-based material has very good photon yield and X-ray cut-off capability, but has long luminous afterglow, which affects the application of the Eu-doped lutetium oxide-based material in dynamic X-ray imaging. On the other hand, the large-size ceramic is very difficult to prepare in a transparentizing way, and high-purity nano powder is usually prepared by a complex wet chemical method, and then the high-transparency material can be obtained by ultra-high temperature sintering. Meanwhile, partial Eu-doped lutetium oxide based materials also have the problem of low light transmittance (< 60%).
Disclosure of Invention
The invention overcomes the defects of the prior art and provides a novel (Eu) x Sc y Lu 1-x-y ) 2 O 3 The transparent scintillator material and the preparation method of the transparent ceramic thereof are expected to simply and rapidly prepare large-size high-transparency Eu and Sc co-doped transparent lutetium oxide-based ceramic.
In order to solve the technical problems, one embodiment of the present invention adopts the following technical scheme:
a process for preparing Eu-Sc co-doped transparent lutetium oxide ceramic includes such steps as calculating the cationic content of ceramic, and mixing europium oxide and scandium oxide according to Eu 3+ The solid solution concentration is 1 to 8at percent, sc 3+ The solid solution concentration is 5-45 at.% doped into lutetium oxide, the doping step comprises the following steps in sequence: ball milling, molding, sintering and annealing the raw materials. Calculated by the cation content in the ceramic, lu 3+ The solid solution concentration is 49-91%.
In the above technical scheme, a more preferable technical scheme is that the preparation method of the Eu and Sc co-doped transparent lutetium oxide ceramic is characterized in that calculated by cation content in the ceramic, europium oxide and scandium oxide are calculated according to Eu 3+ The solid solution concentration is 4 to 6at percent, sc 3+ The solid solution concentration is 10-35 at.% doped into lutetium oxide. Calculated by the cation content in the ceramic, lu 3+ The solid solution concentration is 61-86%.
Further preferred technical proposal is that Eu and Sc are co-dopedThe preparation method of the ceramic is characterized in that calculated by the cation content in the ceramic, europium oxide and scandium oxide are mixed according to Eu 3+ The solid solution concentration is 4 to 6at percent, sc 3+ The solid solution concentration is 25-35 at.% doped into lutetium oxide. Calculated by the cation content in the ceramic, lu 3+ The solid solution concentration is 59-71%.
The prepared Eu and Sc co-doped transparent lutetium oxide ceramic only contains Eu 3+ 、Sc 3+ 、Lu 3+ Three cations.
According to a preferred embodiment of the present invention, eu 3+ The solid solution concentration is 5 to 7at.%, including but not limited to 5.0%, 5.5%, 6.0%, 6.5%, 7.0%.
The doping step of the Eu and Sc co-doped transparent lutetium oxide ceramic adopts the following process conditions:
(1) Adding 4N-purity europium oxide, scandium oxide and lutetium oxide powder into a ball milling tank, using high-purity zirconium oxide ball milling balls as milling balls, using deionized water as a milling medium, and uniformly mixing by a high-energy ball milling method to obtain slurry;
(2) Fully drying the slurry by using an infrared drying oven, and sieving to obtain ceramic powder with good stacking performance;
(3) Drying and pressing the ceramic powder into a wafer, performing cold isostatic pressing under the pressure of 140-200 MPa for further pressing, then heating to 800-1200 ℃ in a muffle furnace at the heating rate of 3-5 ℃/min, preserving heat and calcining for 8-12 h, and then cooling to room temperature at the cooling rate of 3-5 ℃/min; then placing the wafer into a vacuum sintering furnace, and vacuumizing to ensure that the vacuum degree is less than 5 multiplied by 10 -3 Pa, heating to 1650-1750 ℃ at a heating rate of 3-5 ℃/min, calcining for 8-10 h at a heat preservation time, and cooling to room temperature at a cooling rate of 3-5 ℃/min; then placing the ceramic wafer into a hot isostatic pressing sintering furnace, heating to 1600-1700 ℃ at a heating rate of 10 ℃/min, preserving heat and pressure for sintering for 2 hours under 200MPa, and cooling to room temperature at a cooling rate of 10 ℃/min to obtain a preform;
(4) And (3) placing the preform into a muffle furnace for calcination and annealing: raising the temperature to 1300-1400 ℃ at a heating rate of 3 ℃/min, preserving heat for 8-12 h, and then cooling the temperature to room temperature at a cooling rate of 3 ℃/min;
(5) And mechanically polishing the surface of the annealed sample to obtain the Eu and Sc co-doped transparent lutetium oxide ceramic.
In the preparation method, the high-energy ball milling speed in the step (1) is 180-240 rpm; the sieving in the step (2) means sieving with a 100-150 mesh sieve; the average particle size of the europium oxide, scandium oxide and lutetium oxide powder is smaller than 1 micron.
After the ceramic powder is pressed into a wafer, sintering is carried out by adopting a muffle furnace, a vacuum sintering furnace and a hot isostatic pressing sintering furnace. The muffle furnace is used for presintering the ceramic biscuit and removing water and organic components in the biscuit. The vacuum sintering furnace makes the ceramic biscuit complete densification over 95%. And the residual air holes in the ceramic are removed by hot isostatic pressing sintering, so that the transparency of the sample is improved.
The Eu and Sc co-doped transparent lutetium oxide ceramic obtained by the preparation method is also called a transparent scintillator material, the light transmittance at 611nm can reach more than 50%, and the light transmittance of part of products at 611nm exceeds 75%.
Eu and Sc co-doped transparent lutetium oxide ceramic x Sc y Lu 1-x-y ) 2 O 3 And expressing, wherein the value range of x is 0.01-0.08, and the value range of y is 0.05-0.45.
The invention innovatively provides a novel (Eu) x Sc y Lu 1-x-y ) 2 O 3 Lutetium oxide based scintillator materials and methods of making the same. Compared with the existing material system and technology, the invention has the following advantages:
1.(Eu x Sc y Lu 1-x-y ) 2 O 3 compared with the traditional Eu-doped lutetium oxide based material system, the transparent scintillator material has the characteristics of short afterglow time, high luminous efficiency and high transmittance.
2. By solid solution introduction of Eu and Sc ions, new (Eu x Sc y Lu 1-x-y ) 2 O 3 The transparent scintillator ceramic can obviously reduce the sintering of lutetium oxide materialTemperature, the effect of improving transparency is improved, and meanwhile, the preparation process is relatively simplified, so that the preparation cost is reduced.
Drawings
FIG. 1 is a sample of transparent lutetium oxide ceramic prepared in accordance with eighteen examples.
FIG. 2 shows the afterglow test results of transparent lutetium oxide ceramic samples of the present invention at different doping concentrations.
FIG. 3 is a graph showing the results of an X-ray emission spectrum test of transparent lutetium oxide ceramic samples of the present invention having different doping concentrations.
FIG. 4 shows the results of transmittance testing of transparent lutetium oxide ceramic samples of different doping concentrations according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Eighteen examples raw materials were formulated according to the cation content shown in table 1 and transparent lutetium oxide ceramic samples were obtained using the following preparation process conditions:
(1) Adding 4N-purity europium oxide, scandium oxide and lutetium oxide powder into a ball milling tank, adopting high-purity (purity is 99.9%) zirconium oxide ball grinding balls as grinding balls, adopting deionized water as a grinding medium, and uniformly mixing by a high-energy ball milling method (speed is 200 rpm) to obtain slurry;
(2) Fully drying the slurry by using an infrared drying oven, and then sieving the slurry by using a 100-mesh sieve to obtain ceramic powder with good stacking performance;
(3) Drying and pressing the ceramic powder into a wafer, performing cold isostatic pressing under the pressure of 200MPa for further pressing, then heating to 1000 ℃ in a muffle furnace at the heating rate of 4 ℃/min, preserving heat and calcining for 10 hours, and then cooling to room temperature at the cooling rate of 4 ℃/min; then placing the wafer into a vacuum sintering furnace, and vacuumizing to ensure that the vacuum degree is less than 5 multiplied by 10 -3 Pa, heating to 1700 ℃ at a heating rate of 4 ℃/min, preserving heat and calcining for 9 hours, and then cooling at a cooling rate of 4 ℃/minTo room temperature; then placing the ceramic wafer into a hot isostatic pressing sintering furnace, heating to 1650 ℃ at a heating rate of 10 ℃/min, preserving heat and pressure for sintering for 2 hours under 200MPa, and cooling to room temperature at a cooling rate of 10 ℃/min to obtain a preform;
(4) And (3) placing the preform into a muffle furnace for calcination and annealing: raising the temperature to 1350 ℃ at a heating rate of 3 ℃/min, preserving heat for 10 hours, and then lowering the temperature to room temperature at a cooling rate of 3 ℃/min;
(5) And mechanically polishing the surface of the annealed sample to obtain the Eu and Sc co-doped transparent lutetium oxide ceramic sample.
Table 1 transparent ceramic cation content (at%) for eighteen examples
| Examples numbering | Lu | Eu | Sc | Examples numbering | Lu | Eu | Sc |
| 1-1# | 91 | 4 | 5 | 2-1# | 89 | 6 | 5 |
| 1-2# | 86 | 4 | 10 | 2-2# | 84 | 6 | 10 |
| 1-3# | 81 | 4 | 15 | 2-3# | 79 | 6 | 15 |
| 1-4# | 76 | 4 | 20 | 2-4# | 74 | 6 | 20 |
| 1-5# | 71 | 4 | 25 | 2-5# | 69 | 6 | 25 |
| 1-6# | 66 | 4 | 30 | 2-6# | 64 | 6 | 30 |
| 1-7# | 61 | 4 | 35 | 2-7# | 59 | 6 | 35 |
| 1-8# | 56 | 4 | 40 | 2-8# | 54 | 6 | 40 |
| 1-9# | 51 | 4 | 45 | 2-9# | 49 | 6 | 45 |
The samples prepared in eighteen examples are shown in fig. 1, and it can be seen from fig. 1 that each sample has high transparency, and the transparency of each sample is different to some extent, which is related to the doping amounts of Eu and Sc in the ceramic.
Comparative example
By adopting the technological conditions of the embodiment, europium oxide and lutetium oxide powder are used as raw materials to prepare a europium-doped lutetium oxide ceramic sample without Sc co-doping, wherein the europium doping amount is 36% and the lutetium ion content is 64%.
As shown in FIG. 2, the afterglow test results of samples 1-8 # and comparative example are shown in FIG. 2, and it can be seen from the graph that compared with the europium-doped lutetium oxide ceramic sample without Sc co-doping, the introduction of Sc effectively suppresses the peak at 1.2ms and effectively suppresses the C inside the crystal lattice 2 →S 6 The inhibiting effect exists when the doping amount of Sc is 5-45 at%, which shows that the introduction of Sc improves the afterglow performance of europium-doped lutetium oxide scintillating ceramic. And does not change with the increase of Sc doping amount.
Fig. 3 shows the results of an X-ray excitation spectrum test of transparent scintillating ceramics with Sc doping from 5 to 40at%, and it can be seen from fig. 3 that when Sc doping amount is low to 5at%, the strongest X-ray luminescence can be obtained, and more than 10 at% doping reduces luminescence intensity. The luminous efficiency of the Sc doped sample is 1.5-5 times that of the current commercial BGO crystal, the luminous intensity is relatively considerable, the 5at.% Sc doped sample has the strongest luminous intensity, and five times that of the commercial BGO crystal, but the luminous intensity is rapidly reduced at the 5-10 at.% doped position along with the increase of the Sc doping concentration, and then the luminous intensity tends to be gentle, so that the Sc doping amount is not suitable to be excessively large.
Fig. 4 shows the results of transmittance tests for samples 2-1, 3, 4, 6, 8# with a rapid increase in sample transmittance from 17% (@ 611 nm) to 75% (@ 611 nm) over a range of Sc doping of 5-20 at.%. The transmittance reaches the highest 79% (@ 611 nm) when the Sc doping amount is 30at%, and the transmittance is rapidly reduced when the Sc doping amount is increased, and the transmittance of a sample doped with 40at% Sc is only 50% (@ 611 nm). Therefore, the Sc doping amount is not excessively high.
Although the invention has been described herein with reference to illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the scope and spirit of the principles of this disclosure. More specifically, various variations and modifications may be made to the component parts and/or arrangements of the subject combination arrangement within the scope of the disclosure. In addition to variations and modifications in the component parts and/or arrangements, other uses will be apparent to those skilled in the art.
Claims (4)
1. A process for preparing Eu-Sc co-doped transparent lutetium oxide ceramic features that the cationic content in ceramic is calculated, and europium oxide and scandium oxide are used as Eu 3+ The solid solution concentration is 4-6at%, sc 3+ The solid solution concentration is 10-30 at.% and is doped into lutetium oxide, and the doping steps are as follows:
(1) Adding 4N-purity europium oxide, scandium oxide and lutetium oxide powder into a ball milling tank, adopting zirconium oxide ball grinding balls as grinding balls, and deionized water as a grinding medium, and grinding to obtain slurry;
(2) Fully drying the slurry, and sieving to obtain ceramic powder;
(3) Dry-pressing the ceramic powder into a wafer, carrying out cold isostatic pressing under the pressure of 140-200 MPa, then heating to 800-1200 ℃ in a muffle furnace at the heating rate of 3-5 ℃/min, preserving heat and calcining for 8-12 h, and then cooling to room temperature at the cooling rate of 3-5 ℃/min; then placing the wafer into a vacuum sintering furnace, and vacuumizing to ensure that the vacuum degree is less than 5 multiplied by 10 -3 Pa, heating to 1650-1750 ℃ at a heating rate of 3-5 ℃/min, calcining for 8-10 h at a heat preservation time, and cooling to room temperature at a cooling rate of 3-5 ℃/min; then placing the ceramic wafer into a hot isostatic pressing sintering furnace, heating to 1600-1700 ℃ at a heating rate of 10 ℃/min, preserving heat and pressure for sintering for 2 hours under 200MPa, and cooling to room temperature at a cooling rate of 10 ℃/min to obtain a preform;
(4) And (3) placing the preform into a muffle furnace for calcination and annealing: raising the temperature to 1300-1400 ℃ at a heating rate of 3 ℃/min, preserving heat for 8-12 h, and then cooling the temperature to room temperature at a cooling rate of 3 ℃/min;
(5) And mechanically polishing the surface of the annealed sample to obtain the Eu and Sc co-doped transparent lutetium oxide ceramic.
2. The method for preparing Eu/Sc co-doped transparent lutetium oxide ceramic according to claim 1, wherein the remaining cations are Lu only 3+ 。
3. The Eu-Sc co-doped transparent lutetium oxide ceramic obtained by the method of claim 1 or 2.
4. A Eu-Sc co-doped transparent lutetium oxide ceramic according to claim 3, characterized by a light transmission of over 75% at 611 nm.
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| GB0905360D0 (en) * | 2009-03-27 | 2009-05-13 | Cambridge Entpr Ltd | High temperature superconductors |
| JP2015212209A (en) * | 2014-05-02 | 2015-11-26 | 信越化学工業株式会社 | Magnetic optical material and magnetic optical device |
| CN108585853A (en) * | 2017-12-11 | 2018-09-28 | 上海大学 | A kind of europium doping scandium oxide scintillator and its preparation method and application |
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