CN104557012A - Preparation method of Pr:LuAG ceramic scintillator - Google Patents
Preparation method of Pr:LuAG ceramic scintillator Download PDFInfo
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- CN104557012A CN104557012A CN201410797180.0A CN201410797180A CN104557012A CN 104557012 A CN104557012 A CN 104557012A CN 201410797180 A CN201410797180 A CN 201410797180A CN 104557012 A CN104557012 A CN 104557012A
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Abstract
The invention relates to a preparation method of a Pr:LuAG ceramic scintillator. The method comprises the following steps: weighing the raw material powder according to the molar ratio of the required metal elements in (Lu(1-x)Prx)3Al5O12, wherein 0.005<=x<=0.05; adding a sintering aid and performing ball milling; drying the screened powder and calcining in a muffle; moulding, calcining the biscuit and sintering in a vacuum sintering furnace, wherein the vacuum degree is 10<-3>-10<-4>Pa; and finally, annealing the ceramic after the vacuum sintering in a high-temperature muffle to obtain the ceramic scintillator. The light output of the Pr:LuAG ceramic scintillator prepared by the preparation method provided by the invention reaches 16,000-20,000phot/MeV, the energy efficiency is 9-11%, the stopping power on X rays is very strong, and the harm to a human body caused by the X rays is greatly reduced.
Description
Technical field
The present invention relates to a kind of preparation method of Pr:LuAG scintillating ceramic; Particularly relate to a kind of vacuum sintering technology that adopts and prepare doping Pr
3+luetcium aluminum garnet (Pr:Lu
3al
5o
12, Pr:LuAG) the method for scintillating ceramic, obtained photoyield is high, and density is large, and X (γ) ray stopping power is strong, and twilight sunset is little, the scintillating ceramic that energy resolution is good.
Background technology
Along with the development of medical science, X ray computer tomoscan image art (X-CT), Positron emission computed tomography art (PET) are used more and more general, novel high-density, High Light Output, the demand that decay inorganic scintillation material parking stall is urgent soon.Scintillation material is in the market divided into scintillation crystal and scintillating ceramic two kinds.Scintillation crystal is relative to scintillating ceramic, and its growth cycle is long, generally at 10 days to 30 days, require harsher, and it is very difficult to grow the larger crystal of diameter to growing environment; And scintillating ceramic only needs to utilize the existing raw material in market, entered certain processes and just can obtain high-performance, transparent scintillating ceramic.
In recent ten years, AM General electrical equipment (GE) company, Siemens (Simens) and FDAC (Hitachi) company and some research units have carried out the research of medical ceramic scintillator in succession, develop Eu
3+/ Pr
3+: (Y, Gd)
2o
3(YGO), Pr
3+/ Ce
3+/ F
-: Gd
2o
2s:(GSO), Cr
3+/ Ce
3+: Gd
3ga
5o
12(GGG) etc. rear-earth-doped oxide compound, oxysulfide and oxysalt ceramic scintillator, and successfully by YGO, GSO ceramic applications is on medical science X-CT.
It is little that YGO, GSO scintillating ceramic also also exists photoyield, the problem that X-ray stopping power is not strong.Someone proposes to do substrate with LuAG and prepares scintillating ceramic at present.LuAG belongs to isometric system, and spacer is O
h 10-Ia3d, containing 8 chemical combination formula weights in each structure cell, therefore its structure is made up of some interconnected positive tetrahedrons and regular octahedron.The angle of these positive tetrahedrons and regular octahedron is all 0
2-ion, and its center is all Al
3+, these positive tetrahedrons and regular octahedron link up the larger space of formation, and these spaces are aberrated cube body, and its center is by Lu
3+in occupation of.Stable cubic lattice structure and excellent physicochemical property make LuAG become a kind of luminous substrate material of excellent performance.
At employing LuAG as in substrate equipment scintillating ceramic, patent of invention 1 (201210182586.9) adopts the method for co-precipitation and vacuum sintering to prepare Ce:LuAG, it take bicarbonate of ammonia as precipitation agent, with hydroxypropylcellulose (HPC) for dispersion agent.The Ce:LuAG scintillating ceramic light output finally prepared is 12000 ~ 14000phot/MeV, and fall time is nanosecond (30ns).Patent of invention 2 (201110192373.X) list, is prepared for sintering aid with orthosilicic acid tetraethyl ester, and decay is fast, the LuAG scintillating ceramic of the doped with rare-earth elements that density is high.Document 1 (Y.Shi, M.Nikl, X.Feng, etc, J.Appl.Phys 109,013522 (2011)), adopting with 0.5wt%TEOS is sintering aid, is 1700 ~ 1830 DEG C of Pr:LuAG scintillating ceramics preparing that energy resolution is 15% in vacuum sintering temperature.The coprecipitation method method that foregoing invention patent 1 adopts is loaded down with trivial details, and preparation cycle is long, the method that patent of invention 2 and document 2 adopt, and single is sintering aid with TEOS, vacuum sintering temperature high (generally more than 1700 DEG C).
Summary of the invention
The object of the invention is the preparation method providing a kind of Pr:LuAG scintillating ceramic in order to improve the deficiencies in the prior art.
Technical scheme of the present invention is: a kind of (Pr
3+doping Luetcium aluminum garnet) preparation method of Pr:LuAG scintillating ceramic, its concrete steps are:
(1) powder metage, ball milling and drying: by (Lu
1-xpr
x)
3al
5o
12, the metallic element molar ratio weighing material powder needed for 0.005≤x≤0.05 forms, and add sintering aid in ball grinder, add dehydrated alcohol as ball-milling medium simultaneously, ball grinder is put into ball milling on ball mill; Taken out by powder after ball milling, the powder after drying and screening puts into retort furnace calcining;
(2) forming process of ceramics and pre-burning: treat that powder cools, be pressed into biscuit, pressure is 20 ~ 40MPa, then biscuit is carried out isostatic cool pressing, pressure is 160 ~ 250MPa, pressurize 5 ~ 10min; Biscuit after isostatic cool pressing is put into retort furnace calcine, calcining temperature is 800 ~ 1000 DEG C, insulation 5 ~ 10h;
(3) vacuum sintering and annealing: burned biscuit is put into vacuum sintering furnace and sinters, vacuum tightness is 10
-3~ 10
-4pa; Finally the pottery after vacuum sintering is put into high temperature Muffle furnace to anneal, finally through row cutting and polishing, scintillating ceramic is obtained to pottery.
Preferably above-mentioned material powder is for being commercially available high-purity α-Al
2o
3(>99.99%), commercially available high-purity Lu
2o
3(>99.99%), commercially available high-purity Pr
6o
11(>99.99%); Sintering aid is preferably tetraethoxy (TEOS) and boron oxide (B
2o
3); B in co-sintering auxiliary agent
2o
30.01 ~ 0.10% and 0.01 ~ 0.50% of material powder (Pr, Al, Lu raw material) quality summation is respectively with the quality used of TEOS.Ball-milling medium is dehydrated alcohol; Preferred dehydrated alcohol and material powder (Pr, Al, Lu raw material) mass ratio are 1 ~ 3:1.For avoiding impurity to be mixed into, the preferred high purity aluminium oxide ball of abrading-ball, the preferred high purity aluminium oxide tank of ball grinder; Preferred feedstock powder: mass ratio=1:(1 ~ 4 of ball)
In preferred steps (1), rotational speed of ball-mill is 140 ~ 200r/min, and Ball-milling Time is 10 ~ 18h; Drying temperature is 50 ~ 70 DEG C, and time of drying is 10 ~ 12h; In retort furnace, calcining temperature is 600 ~ 900 DEG C, and soaking time is 3 ~ 6h.
In preferred steps (3), vacuum sintering temperature is 1300 ~ 1650 DEG C, insulation 10 ~ 24h; Annealing temperature is 1100 ~ 1500 DEG C, and annealing time is 4-10h.
The present invention is with business α-Al
2o
3(>99.99%), Lu
2o
3and Pr (>99.99%)
6o
11(>99.99%) be raw material, with tetraethoxy (TEOS) and B
2o
3for sintering aid, adopt vacuum sintering technology, on the basis of biscuit of ceramics obtaining the pressed by powder that stability is high, proportioning correct, mix, the scintillating ceramic that obtained photoyield is high, density large, X (γ) ray stopping power is strong, twilight sunset is little, energy resolution is good.
Beneficial effect:
1, the present invention is by adding B simultaneously
2o
3with TEOS as sintering aid, greatly reduce sintering temperature, after adding sintering aid, vacuum sintering is down to 1300 ~ 1650 DEG C.Grain growing is simultaneously abundant, without obvious grain boundary porosity.
2, by the Pr:LuAG scintillating ceramic that preparation method of the present invention prepares, its light output reaches 16000 ~ 20000phot/MeV, and energy efficiency is 9% ~ 11%, very large to the stopping power of X-ray, greatly reduces the injury of X-ray to human body.
Accompanying drawing explanation
Fig. 1 is the SEM figure of powder after 0.5at%Pr:LuAG ball milling in embodiment 1;
Fig. 2 is sample photo before and after the polishing of Pr:LuAG scintillating ceramic in embodiment 1.
Embodiment
After now specific embodiments of the invention being specified in: table 1 is the allocation sheet of three cases.
Table 1
| 1# | 2# | 3# | |
| x | 0.005 | 0.01 | 0.05 |
| Pr 2O 11Quality | 0.449g | 0.898g | 4.507g |
| Lu 2O 3Quality | 104.641g | 104.169g | 100.374g |
| Al 2O 3Quality | 44.910g | 44.933g | 45.119g |
| TEOS quality | 0.015g(0.01wt.％) | 0.45g(0.30wt.％) | 0.75g(0.50wt.％) |
| B 2O 3Quality | 0.15g(0.10wt.％) | 0.1g(0.07wt.％) | 0.015g(0.01wt.％) |
| Dehydrated alcohol quality | 150g(1:1) | 450g(1:3) | 225g(1:1.5) |
| Alumina balls | 150g(1:1) | 600g(1:4) | 300g(1:2) |
Embodiment 1. (preparation 0.5at%Pr:LuAG)
(1) by Lu
2o
3, Al
2o
3, Pr
6o
11according to stoichiometry Lu
2.985pr
0.015al
5o
12carry out proportioning, concrete batching quality is in Table 1#.
(2) put on ball mill by ball grinder, setting rotational speed of ball-mill is 200r/min, ball milling 10h.Raw material after ball milling is taken out, puts into the loft drier of 50 DEG C, dry 12h.Powder after sieving is put into retort furnace calcining 900 DEG C, insulation 3h, the organism brought in removing mechanical milling process.
(4) treat that powder cools, by pressed by powder powder biscuit, hydraulic pressures is 40MPa, then by biscuit through row isostatic cool pressing, pressure is 160MPa, pressurize 10min.Biscuit after cold grade is put into retort furnace calcine, calcining temperature is 1000 DEG C, insulation 5h.
(5) burned biscuit is put into vacuum sintering furnace to sinter, sintering temperature is at 1650 DEG C, and vacuum tightness is 10
-4pa is incubated 10h.Finally the pottery after vacuum sintering is put into high temperature Muffle furnace to anneal, annealing temperature is 1500 DEG C of annealing times is 4h, finally obtains scintillating ceramic to pottery through row cutting and polishing.Scintillating ceramic prepared by this example adopts DEP PPO 475B, Ortec 572spectroscopy amplifier and Ortec927
tMmultichannel analyzer carries out test and measures, and light output reaches 16000phot/MeV, and energy efficiency is 9%, and it is very large to the stopping power of X-ray, greatly reduces the injury of X-ray to human body; Wherein, after ball milling, the SEM figure of powder is shown in Fig. 1, its mixing all with, particle diameter is all less than 300nm, and Fig. 2 is shown in by the photo before and after sample polishing, and after polishing, sample optical quality better, is of a size of 17mm.
Embodiment 2. (preparation 1.0at%Pr:LuAG)
(1) by Lu
2o
3, Al
2o
3, Pr
6o
11according to stoichiometry Lu
2.97pr
0.03al
5o
12carry out proportioning, concrete batching quality is in Table 2#.
(2) put on ball mill by ball grinder, setting rotational speed of ball-mill is 140r/min, ball milling 16h.Raw material after ball milling is taken out, puts into the loft drier of 70 DEG C, dry 10h.Powder after sieving is put into retort furnace calcining 600 DEG C, insulation 6h, the organism brought in removing mechanical milling process.
(4) treat that powder cools, pressed by powder become, powder biscuit, pressure is 20MPa, then by biscuit through row isostatic cool pressing, pressure is 250MPa, pressurize 5min.Biscuit after cold grade is put into retort furnace calcine, calcining temperature is 800 DEG C, insulation 10h.
(5) burned biscuit is put into vacuum sintering furnace to sinter, sintering temperature is at 1300 DEG C, and vacuum tightness is 10
-4pa is incubated 24h.Finally the pottery after vacuum sintering is put into high temperature Muffle furnace to anneal, annealing temperature is 1100 DEG C of annealing times is 10h, finally obtains scintillating ceramic to pottery through row cutting and polishing.Scintillating ceramic light output prepared by this example reaches 18000phot/MeV, and energy efficiency is 10%, it is very large to the stopping power of X-ray, greatly reduces the injury of X-ray to human body.
Embodiment 3. (preparation 5.0at%Pr:LuAG)
(1) by Lu
2o
3, Al
2o
3, Pr
6o
11according to stoichiometry Lu
2.85pr
0.15al
5o
12carry out proportioning, concrete batching quality is in Table 3#.
(2) put on ball mill by ball grinder, setting rotational speed of ball-mill is 200r/min, ball milling 10h.Raw material after ball milling is taken out, puts into the loft drier of 60 DEG C, dry 11h.Powder after sieving is put into retort furnace calcining 800 DEG C, insulation 4h, the organism brought in removing mechanical milling process.
(4) treat that powder cools, pressed by powder is become powder biscuit, pressure is 30MPa, then by biscuit through row isostatic cool pressing, pressure is 200MPa, pressurize 8min.Biscuit after cold grade is put into retort furnace calcine, calcining temperature is 1000 DEG C, insulation 5h.
(5) burned biscuit is put into vacuum sintering furnace to sinter, sintering temperature is at 1500 DEG C, and vacuum tightness is 10
-3pa is incubated 14h.Finally the pottery after vacuum sintering is put into high temperature Muffle furnace to anneal, annealing temperature is 1450 DEG C of annealing times is 5h, finally obtains scintillating ceramic to pottery through row cutting and polishing.Scintillating ceramic light output prepared by this example reaches 20000phot/MeV, and energy efficiency is 11%, and it is very large to the stopping power of X-ray, greatly reduces the injury of X-ray to human body.
Claims (5)
1. a preparation method for Pr:LuAG scintillating ceramic, its concrete steps are:
(1) powder metage, ball milling and drying: by (Lu
1-xpr
x)
3al
5o
12, the metallic element molar ratio weighing material powder needed for 0.005≤x≤0.05 forms, and add sintering aid in ball grinder, add ball-milling medium simultaneously, ball grinder is put into ball milling on ball mill; Taken out by powder after ball milling, the powder after drying and screening puts into retort furnace calcining;
(2) forming process of ceramics and pre-burning: treat that powder cools, be pressed into biscuit, pressure is 20 ~ 40MPa, then biscuit is carried out isostatic cool pressing, pressure is 160 ~ 250MPa, pressurize 5 ~ 10min; Biscuit after isostatic cool pressing is put into retort furnace calcine, calcining temperature is 800 ~ 1000 DEG C, insulation 5 ~ 10h;
(3) vacuum sintering and annealing: burned biscuit is put into vacuum sintering furnace and sinters, vacuum tightness is 10
-3~ 10
-4pa; Finally the pottery after vacuum sintering is put into high temperature Muffle furnace to anneal, finally through row cutting and polishing, scintillating ceramic is obtained to pottery.
2., by preparation method according to claim 1, it is characterized in that described material powder is high-purity α-Al
2o
3, high-purity Lu
2o
3with high-purity Pr
6o
11; Sintering aid is tetraethoxy and boron oxide; Ball-milling medium is dehydrated alcohol; Dehydrated alcohol and material powder mass ratio are 1 ~ 3:1.
3., by preparation method according to claim 2, it is characterized in that B in co-sintering auxiliary agent
2o
30.01 ~ 0.10% and 0.01 ~ 0.50% of material powder quality is respectively with the quality used of TEOS.
4., by preparation method according to claim 1, it is characterized in that in step (1), rotational speed of ball-mill is 140 ~ 200r/min, Ball-milling Time is 10 ~ 18h; Drying temperature is 50 ~ 70 DEG C, and time of drying is 10 ~ 12h; In retort furnace, calcining temperature is 600 ~ 900 DEG C, and soaking time is 3 ~ 6h.
5., by preparation method according to claim 1, it is characterized in that in step (3), vacuum sintering temperature is 1300 ~ 1650 DEG C, insulation 10 ~ 24h; Annealing temperature is 1100 ~ 1500 DEG C, and annealing time is 4-10h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106977204A (en) * | 2015-11-25 | 2017-07-25 | 美国西门子医疗解决公司 | The method that optical interface is generated in pomegranate feldspar |
| CN107324805A (en) * | 2016-04-29 | 2017-11-07 | 中国科学院上海硅酸盐研究所 | A kind of multicomponent garnet-base laser transparent ceramic material and preparation method thereof |
| CN108751991A (en) * | 2018-08-17 | 2018-11-06 | 徐州市江苏师范大学激光科技有限公司 | A kind of laser sintered preparation Tb:Lu2O3The method of ceramics |
| CN111116207A (en) * | 2019-12-19 | 2020-05-08 | 徐州凹凸光电科技有限公司 | Oxynitride fluorescent ceramic material with long-wave-band emission and high color rendering index and preparation method thereof |
| CN111908910A (en) * | 2020-08-18 | 2020-11-10 | 新沂市锡沂高新材料产业技术研究院有限公司 | High-color-rendering-index transparent ceramic for warm white lighting and preparation method thereof |
| CN115490517A (en) * | 2022-10-17 | 2022-12-20 | 闽都创新实验室 | Red light flashing ceramic and preparation method and application thereof |
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| CN102060539A (en) * | 2009-11-13 | 2011-05-18 | 中国科学院上海硅酸盐研究所 | Method for preparing yttrium aluminum garnet based transparent ceramic by slip casting |
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| YIQIANG SHEN ET AL.: "The radiation hardness of Pr:LuAG scintillating ceramics", 《CERAMICS INTERNATIONAL》 * |
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| CN106977204A (en) * | 2015-11-25 | 2017-07-25 | 美国西门子医疗解决公司 | The method that optical interface is generated in pomegranate feldspar |
| CN107324805A (en) * | 2016-04-29 | 2017-11-07 | 中国科学院上海硅酸盐研究所 | A kind of multicomponent garnet-base laser transparent ceramic material and preparation method thereof |
| CN108751991A (en) * | 2018-08-17 | 2018-11-06 | 徐州市江苏师范大学激光科技有限公司 | A kind of laser sintered preparation Tb:Lu2O3The method of ceramics |
| CN108751991B (en) * | 2018-08-17 | 2020-03-13 | 徐州华焰特种陶瓷有限公司 | Preparation of Tb: Lu by laser sintering2O3Method for producing ceramic |
| CN111116207A (en) * | 2019-12-19 | 2020-05-08 | 徐州凹凸光电科技有限公司 | Oxynitride fluorescent ceramic material with long-wave-band emission and high color rendering index and preparation method thereof |
| CN111908910A (en) * | 2020-08-18 | 2020-11-10 | 新沂市锡沂高新材料产业技术研究院有限公司 | High-color-rendering-index transparent ceramic for warm white lighting and preparation method thereof |
| CN115490517A (en) * | 2022-10-17 | 2022-12-20 | 闽都创新实验室 | Red light flashing ceramic and preparation method and application thereof |
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Effective date of registration: 20180912 Address after: 221000 No. 99 Xu Hai Road, Xuzhou economic and Technological Development Zone, Xuzhou, Jiangsu Patentee after: Xuzhou Light Lighting Technology Co., Ltd. Address before: 221009 57 Heping Road, Yunlong District, Xuzhou, Jiangsu Patentee before: XUZHOU JIANGSU NORMAL UNIVERSITY LASER TECHNOLOGY CO., LTD. |