CN114988876A - 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 Eu and Sc co-doped transparent lutetium oxide ceramic and a preparation method thereof 3+ Solid solution concentration is 1-8 at.%, and Sc 3+ Doping lutetium oxide with a solid solution concentration of 5-45 at% 3+ The solid solution concentration is 49-91%. The doping step comprises the following steps in order: ball milling of raw materials, molding, sintering and annealing. Compared with the traditional Eu-doped lutetium oxide-based material system, the Eu and 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 system and a novel preparation method of a scintillator material for high-energy ray detection. More particularly, the present invention relates to a novel (Eu) x Sc y Lu 1-x-y ) 2 O 3 Transparent scintillator ceramics and a preparation method thereof.
Background
Lutetium oxide (Lu) 2 O 3 ) Belongs to a cubic crystal system, has high transmittance in visible and near infrared bands, and has high density of 9.42g/cm 3 The X-ray detector can effectively block X-rays and is applied to the field of high-energy X-ray detection. And doped with europium ion (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 prospect in the fields of homeland security, medical inspection, space detection and the like. However, lutetium oxide materials have very high melting points (over 2400℃.), and it is very difficult to grow crystals, and there is still a lack of reliable technology to obtain Eu-doped lutetium oxide single crystals of large size. 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, can easily realize large size, and is an ideal preparation method of the lutetium oxide scintillating material.
Though the Eu-doped lutetium oxide-based material has good photon yield and X-ray cutoff capability, the Eu-doped lutetium oxide-based material has too long luminescence afterglow, and the application of the Eu-doped lutetium oxide-based material in dynamic X-ray imaging is influenced. On the other hand, the large-size ceramic is very difficult to be prepared in a transparent manner, and high-purity nano powder is usually prepared by a complicated wet chemical method and then is sintered at ultrahigh temperature to obtain a high-transparent material. Meanwhile, part of Eu-doped lutetium oxide-based material also has the problem of low light transmittance (less than 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 ceramics thereof expect to be capable of simply and rapidly preparing large-size and high-transparency Eu and Sc doped transparent lutetium oxide-based ceramics.
In order to solve the technical problem, one embodiment of the present invention adopts the following technical solutions:
a preparation method of Eu and Sc co-doped transparent lutetium oxide ceramic,calculating the content of cations in the ceramic according to the Eu of the europium oxide and the scandium oxide 3+ Solid solution concentration of 1-8 at.%, and Sc 3+ Doping lutetium oxide with a solid solution concentration of 5-45 at.%, wherein the doping step comprises the following steps in sequence: ball milling of raw materials, molding, sintering and annealing. Calculated by the cation content in the ceramic, Lu 3+ The solid solution concentration is 49-91%.
In the above technical solution, a more preferable technical solution is that the preparation method of Eu and Sc co-doped transparent lutetium oxide ceramic is characterized in that the content of cations in the ceramic is calculated, and europium oxide and scandium oxide are added according to Eu 3+ Solid solution concentration is 4-6 at.%, and Sc 3+ The solid solution concentration is 10-35 at.% and is doped into lutetium oxide. Calculated by the cation content in the ceramic, Lu 3+ The solid solution concentration is 61-86%.
The preferable technical scheme is that the preparation method of the Eu and Sc co-doped transparent lutetium oxide ceramic is characterized in that the content of cations in the ceramic is calculated, and europium oxide and scandium oxide are added according to Eu 3+ Solid solution concentration is 4-6 at.%, and 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 kinds of cations.
According to a preferred embodiment of the present invention, Eu 3+ The solid solution concentration is 5-7 at.%, 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, taking a high-purity zirconia ball milling ball as milling beads and 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 then sieving to obtain ceramic powder with good stacking performance;
(3) the ceramic powder is pressed into a wafer in a dry mode, cold isostatic pressing is carried out under the pressure of 140-200 MPa for further pressing, then the temperature is increased to 800-1200 ℃ in a muffle furnace at the heating rate of 3-5 ℃/min, heat preservation and calcination are carried out for 8-12 h, and then the temperature is reduced to the room temperature at the cooling rate of 3-5 ℃/min; then putting the wafer into a vacuum sintering furnace, vacuumizing to ensure that the vacuum degree is less than 5 multiplied by 10 -3 Pa, raising the temperature to 1650-; then placing the ceramic wafer into a hot isostatic pressing sintering furnace, heating to 1600-1700 ℃ at the heating rate of 10 ℃/min, carrying out heat preservation and pressure maintaining sintering at 200MPa for 2h, and cooling to room temperature at the cooling rate of 10 ℃/min to obtain a preform;
(4) and (3) placing the preform into a muffle furnace for calcining and annealing: heating to 1300-1400 ℃ at the heating rate of 3 ℃/min, preserving the heat for 8-12 h, and then cooling to room temperature at the cooling rate of 3 ℃/min;
(5) and mechanically polishing the surface of the sample obtained after annealing to obtain the Eu and Sc co-doped transparent lutetium oxide ceramic.
In the preparation method, the speed of the high-energy ball mill in the step (1) is 180-240 rpm; the sieving in the step (2) is to sieve the mixture through a sieve of 100-150 meshes; the average grain diameter of the europium oxide powder, the scandium oxide powder and the lutetium oxide powder is less than 1 micron.
After the ceramic powder is pressed into a wafer, the wafer is sintered by adopting a muffle furnace, a vacuum sintering furnace and a hot isostatic pressing sintering furnace. The muffle furnace is used for pre-burning the ceramic biscuit and removing water and organic components in the biscuit. The vacuum sintering furnace enables the ceramic biscuit to achieve densification of more than 95%. And the hot isostatic pressing sintering removes residual air holes in the ceramic, and improves the transparency of the sample.
The Eu and Sc co-doped transparent lutetium oxide ceramic obtained by the preparation method is also called as 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 ceramicWith Eu x Sc y Lu 1-x-y ) 2 O 3 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. Through 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 temperature of the lutetium oxide material, improve the transparency effect, simplify the preparation process and reduce the preparation cost.
Drawings
FIG. 1 is a sample of a transparent lutetium oxide ceramic prepared according to eighteen examples.
FIG. 2 is a graph showing afterglow test results of samples of transparent lutetium oxide ceramic of different doping concentrations according to the present invention.
FIG. 3 is a graph showing the results of X-ray emission spectroscopy measurements of samples of transparent lutetium oxide ceramic of varying doping concentrations in accordance with the present invention.
FIG. 4 is a graph showing the results of transmittance tests on samples of transparent lutetium oxide ceramic of different doping concentrations in accordance with the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Eighteen examples the raw materials were formulated according to the cation content shown in table 1 and the following preparation process conditions were used to obtain transparent lutetium oxide ceramic samples:
(1) adding 4N-purity europium oxide, scandium oxide and lutetium oxide powder into a ball milling tank, taking a high-purity (purity is 99.9%) zirconia ball milling ball as milling beads, taking deionized water as a milling medium, and uniformly mixing by a high-energy ball milling method (speed is 200rpm) to obtain slurry;
(2) fully drying the slurry by using an infrared drying oven, and then sieving the dried slurry by using a 100-mesh sieve to obtain ceramic powder with good stacking performance;
(3) dry-pressing the ceramic powder into a wafer, further pressing by cold isostatic pressing under the pressure of 200MPa, then heating to 1000 ℃ in a muffle furnace at the heating rate of 4 ℃/min, carrying out heat preservation and calcination for 10h, and then cooling to room temperature at the cooling rate of 4 ℃/min; then putting the wafer into a vacuum sintering furnace, vacuumizing to ensure that the vacuum degree is less than 5 multiplied by 10 -3 Pa, heating to 1700 ℃ at the heating rate of 4 ℃/min, carrying out heat preservation calcination for 9h, and then cooling to room temperature at the cooling rate of 4 ℃/min; then, putting the ceramic wafer into a hot isostatic pressing sintering furnace, heating to 1650 ℃ at the heating rate of 10 ℃/min, carrying out heat preservation and pressure maintaining sintering at 200MPa for 2h, and then cooling to room temperature at the cooling rate of 10 ℃/min to obtain a preform;
(4) and (3) placing the preform into a muffle furnace for calcining and annealing: heating to 1350 ℃ at the heating rate of 3 ℃/min, preserving the heat for 10h, and then cooling to room temperature at the cooling rate of 3 ℃/min;
(5) and mechanically polishing the surface of the sample obtained after annealing to obtain the Eu and Sc co-doped transparent lutetium oxide ceramic sample.
TABLE 1 cation content (at.%) of the transparent ceramics of eighteen examples
| Example numbering | Lu | Eu | Sc | Example 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 eighteen samples prepared in the example are shown in fig. 1, and as can be seen from fig. 1, each sample has high transparency, and there is a certain difference in transparency between different samples, which is related to the doping amount of Eu and Sc in the ceramic.
Comparative example
By adopting the process conditions of the embodiment, europium oxide and lutetium oxide powder are used as raw materials to prepare a Sc-codoped europium-doped lutetium oxide ceramic sample, wherein the doping amount of europium is 36 percent, and the lutetium ion content is 64 percent.
As shown in FIG. 2, the afterglow test results of samples No. 1-8 and the comparative example are shown in FIG. 2, and it can be seen from the figure that compared with the Sc-free codoped europium-doped lutetium oxide ceramic sample, the introduction of Sc effectively suppresses the peak at 1.2ms, and effectively suppresses C inside the crystal lattice 2 →S 6 The suppression effect exists in the doping amount of Sc from 5 to 45 at.%, which shows that the introduction of Sc improves the afterglow performance of the europium-doped lutetium oxide scintillating ceramic. And does not change with the increase of the Sc doping amount.
Fig. 3 shows the X-ray excitation spectrum test results of transparent scintillating ceramics doped with Sc from 5 to 40 at.%, and it can be seen from fig. 3 that the strongest X-ray luminescence can be obtained when the Sc doping amount is lower than-5 at%, and the luminescence intensity is reduced when the Sc doping amount exceeds 10 at.%. The luminous efficiency of the Sc doped sample is 1.5-5 times that of the current commercial BGO crystal, the luminous intensity is considerable, 5 at.% of Sc doped samples have the strongest luminous intensity which is five times that of the commercial BGO crystal, but with the increase of the Sc doping concentration, the luminous intensity is rapidly reduced at 5-10 at.% of doped positions and then tends to be flat, which indicates that the Sc doping amount is not suitable to be too large.
FIG. 4 shows the transmittance test results of samples 2-1, 3, 4, 6 and 8#, where the transmittance of the sample is rapidly increased from 17% (@611nm) to 75% (@611nm) within the range of 5 to 20 at.% Sc doping. When the amount of Sc doping is 30 at%, the transmittance reaches 79% at maximum (@611nm), and when the amount of Sc doping is increased, the transmittance decreases rapidly, and the transmittance of a sample doped with 40 at% Sc is only 50% (@611 nm). Therefore, the amount of Sc doped should not be too 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 spirit and scope 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 herein. In addition to variations and modifications in the component parts and/or arrangements, other uses will also be apparent to those skilled in the art.
Claims (10)
1. A preparation method of Eu and Sc co-doped transparent lutetium oxide ceramic is characterized in that the content of cations in the ceramic is calculated, and europium oxide and scandium oxide are added according to Eu and Sc 3+ Solid solution concentration is 1-8 at.%, and Sc 3+ Doping lutetium oxide with a solid solution concentration of 5-45 at.%, wherein the doping step comprises the following steps in sequence: ball milling of raw materials, molding, sintering and annealing.
2. The method of claim 1, wherein the cations in the ceramic are used to form a Eu and Sc co-doped transparent lutetium oxide ceramicCalculating the content of europium oxide and scandium oxide according to Eu 3+ Solid solution concentration of 4-6 at.%, and Sc 3+ The solid solution concentration is 10-35 at.% and is doped into lutetium oxide.
3. The method for preparing Eu and Sc co-doped transparent lutetium oxide ceramic according to claim 1, wherein the content of cations in the ceramic is calculated, and europium oxide and scandium oxide are added according to Eu and Sc 3+ Solid solution concentration is 4-6 at.%, and Sc 3+ The solid solution concentration is 25-35 at.% doped into lutetium oxide.
4. The method of preparing Eu and Sc co-doped transparent lutetium oxide ceramic according to claim 1, wherein Lu is calculated as cation content in the ceramic 3+ The solid solution concentration is 49-91%.
5. The method of preparing Eu and Sc co-doped transparent lutetium oxide ceramic according to claim 2, wherein Lu is calculated as cation content in the ceramic 3+ The solid solution concentration is 61-86%.
6. The method of preparing Eu and Sc co-doped transparent lutetium oxide ceramic according to claim 3, wherein Lu is calculated as cation content in the ceramic 3+ The solid solution concentration is 59-71%.
7. The method of preparing an Eu and Sc co-doped transparent lutetium oxide ceramic according to any one of claims 1 to 6, wherein the remaining cations are only Lu 3+ 。
8. The method of preparing a Eu, Sc co-doped transparent lutetium oxide ceramic according to claim 7, wherein the doping step is as follows:
(1) europium oxide, scandium oxide and lutetium oxide powder with the purity of 4N are added into a ball milling tank, zirconia ball milling balls are used as milling beads, deionized water is used as a milling medium, and the mixture is milled to obtain slurry;
(2) fully drying the slurry, and then 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, carrying out heat preservation and calcination for 8-12 h, and then cooling to room temperature at the cooling rate of 3-5 ℃/min; then putting the wafer into a vacuum sintering furnace, vacuumizing to ensure that the vacuum degree is less than 5 multiplied by 10 -3 Pa, raising the temperature to 1650-; then putting the ceramic wafer into a hot isostatic pressing sintering furnace, heating to 1600-1700 ℃ at the heating rate of 10 ℃/min, carrying out heat preservation and pressure maintaining sintering at 200MPa for 2h, and then cooling to room temperature at the cooling rate of 10 ℃/min to obtain a preform;
(4) and (3) placing the preform into a muffle furnace for calcining and annealing: heating to 1300-1400 ℃ at the heating rate of 3 ℃/min, preserving the heat for 8-12 h, and then cooling to room temperature at the cooling rate of 3 ℃/min;
(5) and mechanically polishing the surface of the sample obtained after annealing to obtain the Eu and Sc co-doped transparent lutetium oxide ceramic.
9. Eu, Sc co-doped transparent lutetium oxide ceramic obtainable by the method of any one of claims 1 to 8.
10. The Eu, Sc co-doped transparent lutetium oxide ceramic of claim 9, characterized by a light transmission at 611nm of more than 75%.
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