CN107555977A - Cerium dopping silicic acid lutetium scintillating ceramic and its HIP sintering preparation method - Google Patents
Cerium dopping silicic acid lutetium scintillating ceramic and its HIP sintering preparation method Download PDFInfo
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Abstract
The invention discloses a kind of cerium dopping silicic acid lutetium scintillating ceramic and its HIP sintering preparation method, utilizes dry-pressing formed preparation LSO:Ce biscuits, then biscuit is sintered at a temperature of 1,550 1750 DEG C and obtains the ceramic sintered bodies that relative density is more than 95%, then again by LSO:Ce ceramic sintered bodies carry out high temperature insostatic pressing (HIP)（HIP）Post processing obtains the high ceramic of compact that relative density is up to 99.8%, and translucent LSO is finally obtained after annealing:Ce scintillating ceramics.The LSO:The average grain size of Ce scintillating ceramics is 1.65 μm, in emission wavelength（420nm）Total transmitance at place can reach 58%, and its absolute photoyield is up to 21000photons/MeV, can be used as the material for detector in X ray CT or gamma-rays PET scan imager.
Description
Technical field
The present invention relates to a kind of polycrystalline scintillating ceramic and preparation method thereof, more particularly to a kind of rare earth doped silicic acid
Lutetium scintillating ceramic and preparation method thereof, belong to polycrystalline optical ceramics and its preparing technical field.
Background technology
Cerium dopping silicic acid lutetium (Lu2SiO5:Ce, LSO:Ce it is) to be used for the spokes such as high-energy physics, nuclear medicine and oil well exploration
The key detector material penetrated in field of detecting.Due to Ce3+And Lu3+Ionic radius difference 22% so that Ce3+In LSO:Ce
Crystal ingot in present gradient distribution so that LSO:Ce Scintillation Properties fluctuate.In addition, LSO fusing point is higher than 2050 DEG C,
It is high with the maintenance cost of monocrystal growing furnace in iridium crucible used in single crystal growth process.Using polycrystalline transparent ceramic work
LSO prepared by skill:Ce scintillating ceramics not only overcome problem above, also make LSO:Ce scintillating ceramics remain LSO:Ce monocrystalline materials
The high light yield feature of material, reaches more than the 95% of monocrystalline photoyield, and its short die-away time is suitable with monocrystalline, has excellent flicker
Performance.In order to obtain the polycrystalline optical ceramics of high densification, it is often necessary to which long-time heat preservation realizes cause to discharge stomata at high temperature
Densification.And ceramic material causes always to grow up with significant crystal grain while densification, this can cause aeolotropic crystal structure
The optical transmittance of ceramic material reduces with the increase of crystal grain.
And while can realizing ceramic material densification at a lower temperature using pressure assisted sintering methods, suppress pottery
The grain growth of porcelain, this can significantly increase the optical transmittance of aeolotropic crystal structural ceramic material.U.S. A Erfu
Chen of Randt university (Alfred University) etc. is successfully prepared under 1050 DEG C, 100MPa SPS sintering conditions
Average grain size is 150nm, the Sr of Φ 18.8 × 2mm sizes5(PO4)3F:Yb3+Laser ceramics, the ceramic transmitance are
74%@1000nm.The not bright Hough ceramic technology of Germany and agglomerated material research institute (Fraunhofer Institute for
Ceramic Technologies and Sintered Materials, IKTS) Krell etc. pass through high temperature insostatic pressing (HIP) (HIP) and burn
Knot has obtained crystallite dimension as 0.4-0.6 μm, and straight line transmittance be 55~65%@610nm, size for 100mm × 100mm ×
0.8mm transparent alumina ceramics.
Due to preparing LSO:Ce scintillation single crystals cost is high, prepares that difficulty is big, and preparation process is difficult to control, thus prepare it is low into
The LSO of sheet and high optical property:Ce scintillating ceramics turn into technical problem urgently to be resolved hurrily.
The content of the invention
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind
Cerium dopping silicic acid lutetium scintillating ceramic and its high temperature insostatic pressing (HIP) (HIP) sintering preparation method, using HIP sintering process, ensureing LSO:
The crystallite dimension of ceramics is reduced on the basis of Ce polycrystalline ceramics consistency, this, which is very beneficial for further obtaining, has good printing opacity
The LSO of property:Ce scintillating ceramics.LSO in the present invention:The average grain size of Ce scintillating ceramics is 1.65 μm, is in wavelength
Total transmitance at 420nm emission wavelength can reach more than 58%, and its absolute photoyield is up to 21000photons/MeV, energy
As the material for detector in X ray CT or gamma-rays PET scan imager.The present invention is advantageous to further improve LSO:Ce dodges
The optical transmittance of ceramics is sparkled, such polycrystalline LSO can be effectively facilitated:The practicalization of Ce scintillating ceramics.
To reach above-mentioned purpose, the present invention adopts the following technical scheme that：
A kind of cerium dopping silicic acid lutetium scintillating ceramic, the chemical formula of its material are：(Lu1-xCex)2SiO5:Ce, wherein x=
0.001-0.05。
As currently preferred technical scheme, the grain size range of cerium dopping silicic acid lutetium scintillating ceramic is 0.38-
5.36μm。
As currently preferred technical scheme, with LSO:The density of Ce scintillation single crystal materials is as the close of reference material
Degree, then the relative density of the material of cerium dopping silicic acid lutetium scintillating ceramic is not less than 99.8%.
A kind of HIP sintering preparation method of cerium dopping silicic acid lutetium scintillating ceramic of the present invention, comprises the following steps：
a.LSO:The preparation of Ce biscuits：It is (Lu according to chemical formula1-xCex)2SiO5:Ce target cerium dopping silicic acid lutetium flicker
Ceramic material weighs cerium dopping silicic acid lutetium powder, then pours into cerium dopping silicic acid lutetium powder in stainless steel mould, with 10-
After 40MPa pressure is dry-pressing formed, then the cold isostatic compaction by 100-400MPa, obtain LSO:Ce biscuits；In LSO:Ce
In the preparation process of biscuit, preferably with 20-30MPa pressure it is dry-pressing formed after, further preferably by the cold etc. quiet of 200-250MPa
It is molded, obtain LSO:Ce biscuits；
B. ceramic pre-sintering process：
The LSO that will be prepared in the step a:Ce biscuits, which are put into high temperature sintering furnace, to be sintered, and controls pre-burning junction temperature
Degree system is as follows：
Heated up first, it is 5-10 DEG C/minute that heating rate is controlled below 1200 DEG C；After temperature reaches 1200 DEG C,
1550-1750 DEG C of sintering temperature is raised to 1-5 DEG C/minute of heating rate again, and insulation 2-20 is small under the conditions of sintering temperature
When；After finally reaching 1200 DEG C with 2-10 DEG C/minute of rate of temperature fall, then furnace cooling, it is not low so as to obtain material relative density
In 95% LSO:Ce ceramic sintered bodies, this relative density is with LSO:The density of Ce scintillation single crystal materials is as the close of reference material
Degree；In ceramic pre-sintering process, it is 1600-1700 DEG C preferably to control sintering temperature, and preferably sintering time is 2-4 hours；
C. HIP sintering technique：
To by the pre-sintered LSO prepared of the step b:Ce ceramic sintered bodies are sintered again, control sintering temperature
System is as follows：
Heated up first, controlled below 900 DEG C heating rate be 5-20 DEG C/minute, more than 900 DEG C with 2-10 DEG C/
The heating rate divided continues heating and reaches 1550-1700 DEG C of sintering temperature, and controls the gas of sintering atmosphere in high temperature sintering furnace
Body pressure is 100-190MPa, under this sintering temperature and sintering atmosphere pressure condition, to LSO:Ce ceramic sintered bodies carry out heat
Isostatic sintering PROCESS FOR TREATMENT 1-20 hours, then furnace cooling, obtain LSO:Ce ceramic reinforced sintered bodies；Burnt in high temperature insostatic pressing (HIP)
Tie in technique, it is 1600-1700 DEG C preferably to control sintering temperature, and it is 150-180MPa preferably to control sintering atmosphere pressure, preferably
Sintering time is 2-20 hours；
D. annealing treating process：
Heated up first, it is 5-10 DEG C/minute to control heating rate, and temperature is increased to 1100-1450 DEG C of annealing temperature
Degree, under annealing temperature condition and under air or oxygen atmosphere, the LSO that will be prepared in the step c:Ce ceramic reinforceds are burnt
Knot body carries out making annealing treatment 2-20 hours, finally obtains translucent LSO:Ce scintillating ceramics.In annealing treating process, preferably
It is 1300-1350 DEG C to control annealing temperature, preferably carries out making annealing treatment 4-10 hours.
The present invention compared with prior art, has following obvious prominent substantive distinguishing features and remarkable advantage：
1. the present invention can obtain single-phase, high fine and close LSO by HIP sintering:Ce scintillating ceramics, it is relatively close
Degree is up to 99.8%；
2. the LSO that the present invention obtains:The photoyield of Ce scintillating ceramics can reach LSO:The 95.5% of Ce monocrystalline, its absolute light
Yield can be up to 21000photons/MeV；
3. fine grain LSO prepared by the present invention:The grain size range of Ce ceramics is 0.45-3.50 μm, average grain size
For 1.65 μm, LSO:Total transmitance of the Ce ceramics at 420nm emission wavelength can reach 58%；
4. cerium dopping silicic acid lutetium scintillating ceramic preparation technology of the present invention is simple, easily controllable and implementation.
Brief description of the drawings
Fig. 1 is LSO prepared by the embodiment of the present invention one:The XRD spectrum of Ce ceramics.
Fig. 2 is LSO prepared by the embodiment of the present invention one:The SEM pictures of Ce ceramics.
Fig. 3 is LSO prepared by the embodiment of the present invention one that thickness is 1mm:Total transmittance curve figure of Ce ceramics.
Fig. 4 is LSO prepared by the embodiment of the present invention one:Ce scintillating ceramics exist137Energy spectrum diagram under Cs irradiations.
Embodiment
Details are as follows for the preferred embodiments of the present invention：
Embodiment one：
In the present embodiment, a kind of HIP sintering preparation method of cerium dopping silicic acid lutetium scintillating ceramic, including it is as follows
Step：
a.LSO:The preparation of Ce biscuits：It is (Lu according to chemical formula0.995Ce0.005)2SiO5:Ce target cerium dopping silicic acid lutetium
Flickering ceramic material weighs 2.5g cerium dopping silicic acid lutetium powders, then cerium dopping silicic acid lutetium powder is poured into Φ 20mm cylindrical shape
In stainless steel mould, suppressed with 30MPa pressure, put after then the biscuit after dry-pressing is encapsulated with polybag or rubber sleeve
Enter in cold isostatic press, then the cold isostatic compaction by 200MPa, relative density is obtained up to 53% LSO:Ce biscuits, this phase
To density with LSO:Density of the density of Ce scintillation single crystal materials as reference material；
B. ceramic pre-sintering process：
The LSO that will be prepared in the step a:Ce biscuits, which are put into high temperature Muffle furnace, to be sintered, and controls pre-burning junction temperature
Degree system is as follows：
Heated up first, it is 5 DEG C/minute that heating rate is controlled below 1200 DEG C；After temperature reaches 1200 DEG C, then with
2.5 DEG C/minute of heating rate is raised to 1650 DEG C of sintering temperature, and is incubated 4 hours under the conditions of sintering temperature；Finally with 2 DEG C/
After the rate of temperature fall divided reaches 1200 DEG C, then furnace cooling, so as to obtain the LSO that material relative density is not less than 95%:Ce makes pottery
Porcelain sintered body, this relative density is with LSO:Density of the density of Ce scintillation single crystal materials as reference material；
C. HIP sintering technique：
To by the pre-sintered LSO prepared of the step b:Ce ceramic sintered bodies are sintered again, control sintering temperature
System is as follows：
Heated up first, it is 10 DEG C/minute that heating rate is controlled below 900 DEG C, with 5 DEG C/minute of liter more than 900 DEG C
Warm speed continues heating and reaches 1650 DEG C of sintering temperature, and controls the gas pressure of sintering atmosphere in high temperature sintering furnace to be
150MPa, under this sintering temperature and sintering atmosphere pressure condition, to LSO:Ce ceramic sintered bodies carry out HIP sintering work
Skill is handled 2 hours, then furnace cooling, obtains relative density up to 99.8% LSO:Ce ceramic reinforced sintered bodies；
D. annealing treating process：
Heated up first, it is 5 DEG C/minute to control heating rate, and temperature is increased to 1300 DEG C of annealing temperature, annealed
Under temperature conditionss and in air atmosphere, the LSO that will be prepared in the step c:Ce ceramic reinforceds sintered body is carried out at annealing
Reason 10 hours, to eliminate the Lacking oxygen in ceramics, finally obtain translucent LSO:Ce scintillating ceramics.Cerium manufactured in the present embodiment
The chemical formula for adulterating silicic acid lutetium scintillating ceramic is (Lu0.995Ce0.005)2SiO5:Ce。
The chemical formula of cerium dopping silicic acid lutetium scintillating ceramic manufactured in the present embodiment is (Lu0.995Ce0.005)2SiO5:Ce, cerium are mixed
Miscellaneous silicic acid lutetium (Lu0.995Ce0.005)2SiO5:The grain size range of Ce scintillating ceramics is 0.45-3.50 μm, average grain size
For 1.65 μm.The present embodiment prepares cerium dopping silicic acid lutetium scintillating ceramic using HIP sintering method, can significantly improve this kind of
The optical transmittance of optical anisotropic material.
Experimental test and analysis：
The LSO prepared to embodiment one:It is to use the side of embodiment one that Ce scintillating ceramics, which carry out experiment test and analysis, Fig. 1,
LSO prepared by method:The XRD spectrum of Ce ceramics, embodiment one prepare LSO:The XRD spectrum and mineral crystal diffraction number of Ce ceramics
Matched completely according to the diffraction maximum position and relative intensity of No. 279584 cards in storehouse (ICSD), show single silicic acid lutetium phase.
Fig. 2 is LSO prepared by embodiment one:The SEM pictures of Ce ceramics, LSO prepared by embodiment one:The crystal grain of Ce ceramics
Size range is 0.45-3.50 μm, and average grain size is 1.65 μm.
LSO prepared by embodiment one:Ce ceramics obtain the thick LSO of 1mm after annealing, then after polishing:
Total transmittance curve figure of Ce ceramics is as shown in figure 3, LSO prepared by embodiment one:Ce ceramics are total at 420nm luminous peak positions
Transmitance reaches 58%.Pass through the LSO prepared to embodiment one:The progress in kind of Ce ceramics, which directly visually observes, to be understood, is implemented
The good transparency is presented in ceramics prepared by example one, it is observed that the word of potsherd bottom.Embodiment one is quiet using heat etc.
Pressure aftertreatment technology HIP prepares cerium dopping silicic acid lutetium scintillating ceramic, the LSO:Ce scintillating ceramics exist137Obtained under Cs radiation sources
Energy spectrum diagram as shown in figure 4, its absolute photoyield is 21000photons/MeV, reach LSO:The 95.5% of Ce monocrystalline, can
As the material for detector in X ray CT or gamma-rays PET scan imager, can apply in PET scan imager detector.
Embodiment two：
The present embodiment and embodiment one are essentially identical, are particular in that：
In the present embodiment, a kind of HIP sintering preparation method of cerium dopping silicic acid lutetium scintillating ceramic, including it is as follows
Step：
a.LSO:The preparation of Ce biscuits：It is (Lu according to chemical formula0.95Ce0.05)2SiO5:Ce target cerium dopping silicic acid lutetium
Flickering ceramic material weighs 40g cerium dopping silicic acid lutetium powders, then cerium dopping silicic acid lutetium powder is poured into Φ 50mm cylindrical shape
In stainless steel mould, suppressed with 20MPa pressure, put after then the biscuit after dry-pressing is encapsulated with polybag or rubber sleeve
Enter in cold isostatic press, then the cold isostatic compaction by 250MPa, obtain the LSO that relative density reaches 53-55%:Ce biscuits,
This relative density is with LSO:Density of the density of Ce scintillation single crystal materials as reference material；
B. ceramic pre-sintering process：
The LSO that will be prepared in the step a:Ce biscuits, which are put into high temperature Muffle furnace, to be sintered, and controls pre-burning junction temperature
Degree system is as follows：
Heated up first, it is 5 DEG C/minute that heating rate is controlled below 1200 DEG C；After temperature reaches 1200 DEG C, then with
1.5 DEG C/minute of heating rate is raised to 1700 DEG C of sintering temperature, and is incubated 2 hours under the conditions of sintering temperature；Finally with 2 DEG C/
After the rate of temperature fall divided reaches 1200 DEG C, then furnace cooling, so as to obtain the LSO that material relative density reaches 95-97%:Ce makes pottery
Porcelain sintered body, this relative density is with LSO:Density of the density of Ce scintillation single crystal materials as reference material；
C. HIP sintering technique：
To by the pre-sintered LSO prepared of the step b:Ce ceramic sintered bodies are sintered again, control sintering temperature
System is as follows：
Heated up first, it is 15 DEG C/minute that heating rate is controlled below 900 DEG C, with 8 DEG C/minute of liter more than 900 DEG C
Warm speed continues heating and reaches 1700 DEG C of sintering temperature, and controls the gas pressure of sintering atmosphere in high temperature sintering furnace to be
180MPa, under this sintering temperature and sintering atmosphere pressure condition, to LSO:Ce ceramic sintered bodies carry out HIP sintering work
Skill is handled 2 hours, then furnace cooling, obtains relative density up to 99.8% LSO:Ce ceramic reinforced sintered bodies；
D. annealing treating process：
Heated up first, it is 5 DEG C/minute to control heating rate, and temperature is increased to 1450 DEG C of annealing temperature, annealed
Under temperature conditionss and in air atmosphere, the LSO that will be prepared in the step c:Ce ceramic reinforceds sintered body is carried out at annealing
Reason 4 hours, to eliminate the Lacking oxygen in ceramics, finally obtain translucent LSO:Ce scintillating ceramics.Cerium manufactured in the present embodiment
The chemical formula for adulterating silicic acid lutetium scintillating ceramic is (Lu0.95Ce0.05)2SiO5:Ce。
The good transparency is presented in ceramics manufactured in the present embodiment, and the present embodiment uses post-hiped technique HIP
Prepare cerium dopping silicic acid lutetium scintillating ceramic, the LSO:The grain size range of Ce scintillating ceramics is 0.95-4.70 μm, average crystalline substance
Particle size is 2.75 μm.LSO manufactured in the present embodiment:Total transmitance of the Ce ceramics at 420nm luminous peak positions reaches 55%.
By to LSO manufactured in the present embodiment:The progress in kind of Ce ceramics, which directly visually observes, to be understood, prepared by the present embodiment
Ceramics the good transparency is presented, it is observed that the word of potsherd bottom.LSO manufactured in the present embodiment:Ce flicker potteries
Porcelain exists137Absolute photoyield under Cs radiation sources is 21300photons/MeV, reaches LSO:The 97% of Ce monocrystalline, it can use
Make the material for detector in X ray CT or gamma-rays PET scan imager, can apply in PET scan imager detector.
Embodiment three：
The present embodiment is substantially the same as in the previous example, and is particular in that：
In the present embodiment, a kind of HIP sintering preparation method of cerium dopping silicic acid lutetium scintillating ceramic, including it is as follows
Step：
a.LSO:The preparation of Ce biscuits：It is (Lu according to chemical formula0.999Ce0.001)2SiO5:Ce target cerium dopping silicic acid lutetium
Flickering ceramic material weighs 2.5g cerium dopping silicic acid lutetium powders, then cerium dopping silicic acid lutetium powder is poured into Φ 20mm cylindrical shape
In stainless steel mould, suppressed with 10MPa pressure, put after then the biscuit after dry-pressing is encapsulated with polybag or rubber sleeve
Enter in cold isostatic press, then the cold isostatic compaction by 100MPa, relative density is obtained up to 53% LSO:Ce biscuits, this phase
To density with LSO:Density of the density of Ce scintillation single crystal materials as reference material；
B. ceramic pre-sintering process：
The LSO that will be prepared in the step a:Ce biscuits, which are put into high temperature Muffle furnace, to be sintered, and controls pre-burning junction temperature
Degree system is as follows：
Heated up first, it is 10 DEG C/minute that heating rate is controlled below 1200 DEG C；After temperature reaches 1200 DEG C, then
1550 DEG C of sintering temperature is raised to 1 DEG C/minute of heating rate, and 20 hours are incubated under the conditions of sintering temperature；Finally with 2
DEG C/minute rate of temperature fall reach 1200 DEG C after, then furnace cooling, so as to obtain the LSO that material relative density reaches 95%:Ce makes pottery
Porcelain sintered body, this relative density is with LSO:Density of the density of Ce scintillation single crystal materials as reference material；
C. HIP sintering technique：
To by the pre-sintered LSO prepared of the step b:Ce ceramic sintered bodies are sintered again, control sintering temperature
System is as follows：
Heated up first, it is 5 DEG C/minute that heating rate is controlled below 900 DEG C, with 2 DEG C/minute of liter more than 900 DEG C
Warm speed continues heating and reaches 1600 DEG C of sintering temperature, and controls the gas pressure of sintering atmosphere in high temperature sintering furnace to be
190MPa, under this sintering temperature and sintering atmosphere pressure condition, to LSO:Ce ceramic sintered bodies carry out HIP sintering work
Skill is handled 1 hour, then furnace cooling, obtains relative density up to 99.8% LSO:Ce ceramic reinforced sintered bodies；
D. annealing treating process：
Heated up first, it is 10 DEG C/minute to control heating rate, and temperature is increased to 1100 DEG C of annealing temperature, moved back
Under fiery temperature conditionss and in air atmosphere, the LSO that will be prepared in the step c:Ce ceramic reinforced sintered bodies are annealed
Processing 20 hours, to eliminate the Lacking oxygen in ceramics, finally obtain translucent LSO:Ce scintillating ceramics.It is manufactured in the present embodiment
The chemical formula of cerium dopping silicic acid lutetium scintillating ceramic is (Lu0.999Ce0.001)2SiO5:Ce。
The good transparency is presented in ceramics manufactured in the present embodiment, and the present embodiment uses post-hiped technique HIP
Prepare cerium dopping silicic acid lutetium scintillating ceramic, the LSO:The grain size range of Ce scintillating ceramics is 0.38-3.03 μm, average crystalline substance
Particle size is 1.27 μm.LSO manufactured in the present embodiment:Total transmitance of the Ce ceramics at 420nm luminous peak positions reaches 58%.
By to LSO manufactured in the present embodiment:The progress in kind of Ce ceramics, which directly visually observes, to be understood, prepared by the present embodiment
Ceramics the good transparency is presented, it is observed that the word of potsherd bottom.LSO manufactured in the present embodiment:Ce flicker potteries
Porcelain exists137Absolute photoyield under Cs radiation sources is 21500photons/MeV, reaches LSO:The 97.7% of Ce monocrystalline, can
As the material for detector in X ray CT or gamma-rays PET scan imager, can apply in PET scan imager detector.
Example IV：
The present embodiment is substantially the same as in the previous example, and is particular in that：
In the present embodiment, a kind of HIP sintering preparation method of cerium dopping silicic acid lutetium scintillating ceramic, including it is as follows
Step：
a.LSO:The preparation of Ce biscuits：It is (Lu according to chemical formula0.999Ce0.001)2SiO5:Ce target cerium dopping silicic acid lutetium
Flickering ceramic material weighs 40g cerium dopping silicic acid lutetium powders, then cerium dopping silicic acid lutetium powder is poured into Φ 50mm cylindrical shape
In stainless steel mould, suppressed with 40MPa pressure, put after then the biscuit after dry-pressing is encapsulated with polybag or rubber sleeve
Enter in cold isostatic press, then the cold isostatic compaction by 400MPa, relative density is obtained up to 59% LSO:Ce biscuits, this phase
To density with LSO:Density of the density of Ce scintillation single crystal materials as reference material；
B. ceramic pre-sintering process：
The LSO that will be prepared in the step a:Ce biscuits, which are put into high temperature Muffle furnace, to be sintered, and controls pre-burning junction temperature
Degree system is as follows：
Heated up first, it is 10 DEG C/minute that heating rate is controlled below 1200 DEG C；After temperature reaches 1200 DEG C, then
1750 DEG C of sintering temperature is raised to 5 DEG C/minute of heating rate, and 2 hours are incubated under the conditions of sintering temperature；Finally with 10
DEG C/minute rate of temperature fall reach 1200 DEG C after, then furnace cooling, so as to obtain the LSO that material relative density reaches 97-98%:
Ce ceramic sintered bodies, this relative density is with LSO:Density of the density of Ce scintillation single crystal materials as reference material；
C. HIP sintering technique：
To by the pre-sintered LSO prepared of the step b:Ce ceramic sintered bodies are sintered again, control sintering temperature
System is as follows：
Heated up first, it is 20 DEG C/minute that heating rate is controlled below 900 DEG C, with 10 DEG C/minute more than 900 DEG C
Heating rate continues heating and reaches 1700 DEG C of sintering temperature, and controls the gas pressure of sintering atmosphere in high temperature sintering furnace to be
100MPa, under this sintering temperature and sintering atmosphere pressure condition, to LSO:Ce ceramic sintered bodies carry out HIP sintering work
Skill is handled 20 hours, then furnace cooling, obtains relative density up to 99.9% LSO:Ce ceramic reinforced sintered bodies；
D. annealing treating process：
Heated up first, it is 10 DEG C/minute to control heating rate, and temperature is increased to 1400 DEG C of annealing temperature, moved back
Under fiery temperature conditionss and in air atmosphere, the LSO that will be prepared in the step c:Ce ceramic reinforced sintered bodies are annealed
Processing 20 hours, to eliminate the Lacking oxygen in ceramics, finally obtain translucent LSO:Ce scintillating ceramics.It is manufactured in the present embodiment
The chemical formula of cerium dopping silicic acid lutetium scintillating ceramic is (Lu0.999Ce0.001)2SiO5:Ce。
The good transparency is presented in ceramics manufactured in the present embodiment, and the present embodiment uses post-hiped technique HIP
Prepare cerium dopping silicic acid lutetium scintillating ceramic, the LSO:The grain size range of Ce scintillating ceramics is 1.45-5.36 μm, average crystalline substance
Particle size is 3.78 μm.LSO manufactured in the present embodiment:Total transmitance of the Ce ceramics at 420nm luminous peak positions reaches 54%.
By to LSO manufactured in the present embodiment:The progress in kind of Ce ceramics, which directly visually observes, to be understood, prepared by the present embodiment
Ceramics the good transparency is presented, it is observed that the word of potsherd bottom.LSO manufactured in the present embodiment:Ce flicker potteries
Porcelain exists137Absolute photoyield under Cs radiation sources is 21100photons/MeV, reaches LSO:The 96% of Ce monocrystalline, it can use
Make the material for detector in X ray CT or gamma-rays PET scan imager, can apply in PET scan imager detector.
The embodiment of the present invention is illustrated above in conjunction with accompanying drawing, but the invention is not restricted to above-described embodiment, can be with
A variety of changes are made according to the purpose of the innovation and creation of the present invention, under all Spirit Essence and principle according to technical solution of the present invention
Change, modification, replacement, combination or the simplification made, should be equivalent substitute mode, as long as meeting the goal of the invention of the present invention,
Without departing from technical principle and the invention of cerium dopping silicic acid lutetium scintillating ceramic of the present invention and its HIP sintering preparation method
Design, belongs to protection scope of the present invention.
Claims (8)
- A kind of 1. cerium dopping silicic acid lutetium scintillating ceramic, it is characterised in that：The chemical formula of its material is：(Lu1-xCex)2SiO5:Ce, Wherein x=0.001-0.05.
- 2. cerium dopping silicic acid lutetium scintillating ceramic according to claim 1, it is characterised in that：Cerium dopping silicic acid lutetium scintillating ceramic Grain size range is 0.38-5.36 μm.
- 3. cerium dopping silicic acid lutetium scintillating ceramic according to claim 1 or claim 2, it is characterised in that：With LSO:Ce scintillation single crystal materials Density of the density of material as reference material, then the relative density of the material of cerium dopping silicic acid lutetium scintillating ceramic be not less than 99.8%.
- A kind of 4. HIP sintering preparation method of cerium dopping silicic acid lutetium scintillating ceramic described in claim 1, it is characterised in that Comprise the following steps：a.LSO:The preparation of Ce biscuits：It is (Lu according to chemical formula1-xCex)2SiO5:Ce target cerium dopping silicic acid lutetium scintillating ceramic Material measures cerium dopping silicic acid lutetium powder, then pours into cerium dopping silicic acid lutetium powder in stainless steel mould, with 10-40MPa's After pressure is dry-pressing formed, then the cold isostatic compaction by 100-400MPa, obtain LSO:Ce biscuits；B. ceramic pre-sintering process：The LSO that will be prepared in the step a:Ce biscuits, which are put into high temperature sintering furnace, to be sintered, and controls pre-sintering temperature system Degree is as follows：Heated up first, it is 5-10 DEG C/minute that heating rate is controlled below 1200 DEG C；After temperature reaches 1200 DEG C, then with 1-5 DEG C/minute of heating rate is raised to 1550-1750 DEG C of sintering temperature, and is incubated 2-20 hours under the conditions of sintering temperature；Most After reaching 1200 DEG C afterwards with 2-10 DEG C/minute of rate of temperature fall, then furnace cooling, so as to obtain material relative density not less than 95% LSO:Ce ceramic sintered bodies, this relative density is with LSO:Density of the density of Ce scintillation single crystal materials as reference material；C. HIP sintering technique：To by the pre-sintered LSO prepared of the step b:Ce ceramic sintered bodies are sintered again, control sintering temperature system It is as follows：Heated up first, it is 5-20 DEG C/minute that heating rate is controlled below 900 DEG C, with 2-10 DEG C/minute more than 900 DEG C Heating rate continues heating and reaches 1550-1700 DEG C of sintering temperature, and controls the gas pressure of sintering atmosphere in high temperature sintering furnace Power is 100-190MPa, under this sintering temperature and sintering atmosphere pressure condition, to LSO:It is quiet that Ce ceramic sintered bodies carry out heat etc. Sintering process processing 1-20 hours are pressed, then furnace cooling, obtain LSO:Ce ceramic reinforced sintered bodies；D. annealing treating process：Heated up first, it is 5-10 DEG C/minute to control heating rate, and temperature is increased to 1100-1450 DEG C of annealing temperature, Under annealing temperature condition and under air or oxygen atmosphere, the LSO that will be prepared in the step c:Ce ceramic reinforced sintered bodies Carry out making annealing treatment 2-20 hours, finally obtain translucent LSO:Ce scintillating ceramics.
- 5. HIP sintering preparation method according to claim 4, it is characterised in that：In the LSO of the step a:Ce elements In the preparation process of base, with 20-30MPa pressure it is dry-pressing formed after, then the cold isostatic compaction by 200-250MPa obtains LSO:Ce biscuits.
- 6. HIP sintering preparation method according to claim 4, it is characterised in that：It is pre-sintered in step b ceramics In technique, it is 1600-1700 DEG C to control sintering temperature, and sintering time is 2-4 hours.
- 7. HIP sintering preparation method according to claim 4, it is characterised in that：Burnt in the step c high temperature insostatic pressing (HIP)s Tie in technique, it is 1600-1700 DEG C to control sintering temperature, and it is 150-180MPa, sintering time 2- to control sintering atmosphere pressure 20 hours.
- 8. HIP sintering preparation method according to claim 4, it is characterised in that：Work is made annealing treatment in the step d In skill, it is 1300-1350 DEG C to control annealing temperature, carries out making annealing treatment 4-10 hours.
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| CN109053175A (en) * | 2018-09-28 | 2018-12-21 | 浙江梵彼斯特轻纺发展有限公司 | A kind of cerium dopping lutetium pyrosilicate scintillating ceramic and preparation method thereof |
| CN109053175B (en) * | 2018-09-28 | 2021-05-07 | 浙江梵彼斯特轻纺发展有限公司 | Cerium-doped lutetium disilicate scintillation ceramic and preparation method thereof |
| CN109704783A (en) * | 2018-12-26 | 2019-05-03 | 常熟市银洋陶瓷器件有限公司 | A kind of forming method suitable for thin-wall part output window ceramics |
| CN112062472A (en) * | 2020-08-31 | 2020-12-11 | 华南理工大学 | Lu with high crystallinity and high hardness2Si2O7Transparent microcrystalline glass and preparation method thereof |
| CN112062472B (en) * | 2020-08-31 | 2021-12-17 | 华南理工大学 | High-hardness Lu2Si2O7Transparent microcrystalline glass and preparation method thereof |
| CN112030028A (en) * | 2020-09-03 | 2020-12-04 | 北京安颂科技有限公司 | Aluminum oxide-based metal composite ceramic, preparation method thereof, aluminum oxide-based metal composite ceramic bone implantation prosthesis and application |
| CN112030028B (en) * | 2020-09-03 | 2022-03-01 | 北京安颂科技有限公司 | Aluminum oxide-based metal composite ceramic, preparation method thereof, aluminum oxide-based metal composite ceramic bone implantation prosthesis and application |
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