CN109053175A - A kind of cerium dopping lutetium pyrosilicate scintillating ceramic and preparation method thereof - Google Patents
A kind of cerium dopping lutetium pyrosilicate scintillating ceramic and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to optical ceramics technical fields.Impurity is readily incorporated to solve currently available technology scintillating ceramic, ceramic particle is easy to reunite, and be easy to cause product dispersed, the bad disadvantage of uniformity, a kind of cerium dopping lutetium pyrosilicate scintillating ceramic is proposed, a kind of composition general formula of cerium dopping lutetium pyrosilicate scintillating ceramic of the present invention is (Lu1‑ xCex)2Si2O7, wherein x=0.001-0.06.Present invention employs cerium dopping lutetium pyrosilicate rather than at present raw material of the widely used cerium dopping silicic acid lutetium as scintillating ceramic, improve the scintillation efficiency of product, reduce fusing point, improve luminance temperature, improve applicability of the invention, the transparency and stability of the invention are enhanced simultaneously, therefore the present invention has and intensity height, good insulating, purity is high, uniformity is strong, scintillation properties with advantage resistant to high temperature, can be applied to the mechanical industry CT of special fibre, the technical fields such as clothes fiber measurement by force.
Description
Technical field
The present invention relates to optical ceramics technical field, in particular to a kind of cerium dopping lutetium pyrosilicate scintillating ceramic and its
Preparation method.
Background technique
Ceramic scintillation materials have high density, and High Light Output, high light yield, die-away time is short, are suitable for medical imaging, sky
Between the fields such as physics, high-energy physics, industrial flaw detection, geological prospecting, intelligent clothing field is gradually developed at present, and scintillating ceramic exists
Wherein played an important role, component metal defect detection and special fibre in terms of have important value.
Although ceramic scintillation materials light output is not so good as crystal scintillation material, ceramic scintillation materials generally have good
Bright property and stability, intensity is high, good insulating, being capable of high temperature resistant, corrosion-resistant.Ceramic scintillation materials production is time-consuming short, to equipment
Constraint and limitation of less demanding at low cost, keeping its development more like that with the no crystal scintillation material of application.Ceramic scintillation materials
Since structure is regular unlike requiring crystalline material, so it can preferably realize uniformly mixing for various concentration exciting agent
Miscellaneous, this can be good at the luminescent properties for improving scintillation material.The purity of scintillating ceramic powder, dispersibility, the doping of the second phase are equal
Even property etc. is to influence the key factor of ceramic post sintering performance, and determine the critical issue of scintillating ceramic performance.
Application No. is the patents of invention of CN201210249353.6 to disclose the hot pressed sintering preparation of cerium fluoride scintillating ceramic
Method and its cerium fluoride scintillating ceramic of preparation, to the high-purity CeF being placed in hot pressing die under authorized pressure3Powder carries out pre-
Pressure, high-purity CeF3The purity of powder is 99% or more；Heating process: after shedding preload pressure, vacuumizing reaches vacuum degree
<5×10-3Pa then heats to 800 ~ 1000 DEG C；And hot pressed sintering process: keeping at 800 ~ 1000 DEG C, it is forced into 100 ~
300MPa keeps 0.5 ~ 2.5h of the temperature and pressure, and the ceramics are high with visible light transmittance, crystal grain is small, consistency is high, oxidation
The advantages such as degree is low, but since it there are impurity, ceramic particle is readily incorporated is easy to reunite, product is be easy to cause to disperse
Property, the bad disadvantage of uniformity, therefore the present invention provides a kind of purity is high, uniformity is strong, and the strong cerium dopping of scintillation properties is burnt
Silicic acid lutetium scintillating ceramic and preparation method thereof.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of purity is high, uniformity is strong, and the strong cerium dopping of scintillation properties is burnt
Silicic acid lutetium scintillating ceramic and preparation method thereof.
The composition general formula of a kind of cerium dopping lutetium pyrosilicate scintillating ceramic, the cerium dopping lutetium pyrosilicate scintillating ceramic is
(Lu1-xCex)2Si2O7, wherein x=0.001-0.06.
Present invention employs cerium dopping lutetium pyrosilicate rather than widely used cerium dopping silicic acid lutetium is as flashing at present
The raw material of ceramics mixes cerium lutetium pyrosilicate for octahedra crystalline form, and in the crystal structure with the space C2/m group structure, Lu occupies one
A lattice site, after being replaced by Ce, only one centre of luminescence.And Ce ion is wanted in the space the C2/c group structure of LSO
Two lattice sites are accounted for, therefore there are two the centres of luminescence for LSO tool.It is luminous intensity according to l=- dn/dt(l, n is the centre of luminescence
Number, t is the time), the solid in contrast present invention is with stronger luminous intensity, and cerium dopping lutetium pyrosilicate is that unimolecule is sent out
Light, therefore without twilight sunset, there is better scintillation efficiency compared with cerium dopping silicic acid lutetium.And cerium dopping lutetium pyrosilicate fusing point is low, shines
Temperature is high, has better applicability compared to cerium dopping silicic acid lutetium.
Preferably, general formula (the Lu1-xCex)2Si2O7In Ce3+Ion is active ions.
The present invention uses Ce3+As excited ion, active ions Ce3+Into in lutetium pyrosilicate octahedron, replace Lu3+From
Scintillation properties of the invention can be improved in son, improve luminous efficiency.
A kind of preparation method of cerium dopping lutetium pyrosilicate scintillating ceramic, comprising the following steps:
A is (Lu according to chemical formula1-xCex)2Si2O7Proportion preparation LPS:Ce powder, by LPS:Ce powder and ethyl alcohol according to 1:(1
~4) volume ratio mixing, obtains mixed slurry, mixed slurry is carried out ball milling；
B. 200 ~ 300 meshes will be crossed after the slurry ball milling after ball milling, be then injected into mold and carry out moulding, then in 400-1000
It is calcined under air or oxygen atmosphere at DEG C；
C. preliminary sintering: base at the beginning of the LPS:Ce powder obtained after calcining obtains LPS:Ce after pressure forming；By base at the beginning of LPS:Ce
It is sintered under an argon atmosphere；
D. it double sintering: will be sintered again under an argon atmosphere by the first base being tentatively sintered；
E. annealing process: control heating rate is 5-20 DEG C/min, temperature is increased to 1200-1300 DEG C, in air atmosphere
Anneal 4-10h, obtains cerium dopping lutetium pyrosilicate scintillating ceramic.
Firstly, LPS:Ce powder can be improved and make epigranular present invention employs the scheme of ethyl alcohol mixing and ball milling, from
And the uniformity of product is improved, and the optical property of product is improved, in addition present invention employs the calcining under oxygen or air environment,
The content for facilitating impurity in reduction LPS:Ce powder, improves the purity of product, and the present invention additionally uses two-step sintering, leads to
The stomata on preliminary sintering exclusion material is crossed, then completes the sintering of ceramics by double sintering, to improve the compactness extent of product,
To improve the glitter of product.
Preferably, the LPS:Ce powder is prepared using following steps: by Lu2O3Powder, SiO2Powder, Ce2O3Powder
End is according to general formula (Lu1-xCex)2Si2O7In ion molar ratio example be uniformly mixed, the briquet under 180-200MPa pressure,
Then it puts block into horse kettle furnace, 10-12h is sintered at 1200-1300 DEG C at polycrystalline LPS crystal, by the polycrystalline LPS
Crystal pulverizes and sieves, and obtains LPS:Ce powder.
The present invention is used and is suppressed under High Voltage each component, is improved the rate of reaction, is accelerated the speed of crystal growth, adopt
The speed of production of product is helped to improve with polycrystalline LPS crystal, reduces production cost.
Preferably, the LPS:Ce powder is prepared using following steps: by Lu2O3Powder, SiO2Powder, Ce2O3Powder
End is according to general formula (Lu1-xCex)2Si2O7In ion molar ratio example be uniformly mixed, the briquet under 180-200MPa pressure,
Then it puts block into horse kettle furnace, 10-12h is sintered at 1200-1300 DEG C at polycrystalline LPS crystal, then by polycrystalline LPS crystal
It is dosed into iridium crucible, in pure nitrogen gas or argon atmosphere, crystal carries out pulling growth, monocrystalline LPS crystal is obtained, by the list
Brilliant LPS crystal pulverizes and sieves, and obtains LPS:Ce powder.
Preferably, the revolving speed of crystal is 10-20r/min during the lifting, the speed-raising of crystal is 0.2-
0.3mm/h。
Crystal is carried out pulling growth after obtaining polycrystalline LPS crystal by polycrystalline by the present invention, is obtained monocrystalline LPS crystal, is adopted
Facilitated to reduce the defects of crystal with this method, and there is higher purity and light transmission using the LPS crystal of this method preparation
Ability helps to improve the uniformity and scintillation properties of product.
Preferably, the step of described pressure forming are as follows: first carry out dry-pressing, the pressure of the dry-pressing to LPS:Ce powder
By force be 18-20MPa, after isostatic cool pressing is carried out to the LPS:Ce Jing Guo dry-pressing again, the pressure of the isostatic cool pressing is 100-
LPS:Ce just base is obtained after 200MPa, the temperature being tentatively sintered is 1300 DEG C -2000 DEG C, and the preliminary sintering uses
Argon atmosphere, sintering time 3-4h.
Present invention employs dry-pressing and isostatic cool pressing, and the compactness of product can be enhanced by pressure forming twice, so that
Product has good optical property and scintillation properties, while can promote the mechanical performance of product.
Preferably, the pressure of argon gas is in 350 DEG C of temperature-rise periods below during the double sintering
40-50MPa;In 350 to 800 DEG C of temperature-rise period, heating rate is 10-11 DEG C/min, to 800 DEG C or more of temperature-rise period
In, heating rate is 5-6 DEG C/min, until 1900-2000 DEG C of in-furnace temperature arrival, stops 2- under the conditions of this temperature and pressure
After 3h, 50 ~ 60 DEG C are cooled to the furnace.
Preferably, the pressure of gas gradually increases in 350 DEG C or more of temperature-rise period, the pressure is advanced the speed
For 30-40MPa/h.
The pressure for gradually reinforcing gas during heating and calcining in the present invention program, by inert gas to material
Uniformly applied pressure facilitates grain boundaries and generates sliding under pressure, so that air hole structure is effectively removed, to mention
The compactness of high product so that product has good optical property and scintillation properties, while can promote the mechanicalness of product
Energy.
The beneficial effects of the present invention are the present invention to have the good transparency and stability, and intensity is high, good insulating,
Simultaneously there is purity is high, uniformity is strong, scintillation properties by force and advantage resistant to high temperature.The present invention has the good transparency and stablizes
Property, and intensity is high, good insulating, while having purity is high, and uniformity is strong, scintillation properties by force and advantage resistant to high temperature, Ke Yiying
For the industry CT of intelligent clothing machinery, the technical fields such as clothes fiber measurement.
Specific embodiment
The present invention is further explained With reference to embodiment:
Embodiment 1
The composition general formula of a kind of cerium dopping lutetium pyrosilicate scintillating ceramic, cerium dopping lutetium pyrosilicate scintillating ceramic is
(Lu0.999Ce0.001)2Si2O7, Ce3+Ion is active ions.
A kind of preparation method of cerium dopping lutetium pyrosilicate scintillating ceramic, comprising the following steps:
A is by Lu2O3Powder, SiO2Powder, Ce2O3Powder is according to general formula (Lu0.999Ce0.001)2Si2O7In ion molar ratio example it is mixed
It closes uniformly, then the briquet under 180MPa pressure puts block into horse kettle furnace, 10h is sintered at 1200 DEG C into polycrystalline
Polycrystalline LPS crystal is pulverized and sieved, obtains LPS:Ce powder by LPS crystal, by LPS:Ce powder and ethyl alcohol according to the volume ratio of 1:1
Mixing, obtains mixed slurry, mixed slurry is carried out ball milling；
B. the slurry after ball milling will be crossed 200 ~ 300 meshes, is then injected into mold and carries out moulding, then the sky at 400 DEG C
It is calcined under gas or oxygen atmosphere；
C. preliminary sintering: first carrying out dry-pressing to the LPS:Ce powder obtained after calcining, and the pressure of dry-pressing is 18MPa, after again to warp
The LPS:Ce for crossing dry-pressing carries out isostatic cool pressing, and the pressure of isostatic cool pressing obtains LPS:Ce just base, is tentatively sintered after being 100MPa
Temperature is 1300 DEG C, and using argon atmosphere, sintering time obtains LPS:Ce just base after being 3h for preliminary sintering,
D. double sintering: the pressure of argon gas is 40MPa in 350 DEG C of temperature-rise periods below;350 to 800 DEG C of temperature-rise period
In, heating rate is 10 DEG C/min, and into 800 DEG C or more of temperature-rise periods, heating rate is 5 DEG C/min, until in-furnace temperature
1900 DEG C are reached, after stopping 2h under the conditions of this temperature and pressure, 50 DEG C are cooled to the furnace, in 350 DEG C or more of temperature-rise period
The pressure of middle gas gradually increases, and pressure is advanced the speed as 30MPa/h；
E. annealing process: control heating rate is 5 DEG C/min, temperature is increased to 1300 DEG C, anneal 4h in air atmosphere.
Embodiment 2
A kind of cerium dopping lutetium pyrosilicate scintillating ceramic, the composition general formula of cerium dopping lutetium pyrosilicate scintillating ceramic are (Lu0.94Ce0.06)2Si2O7, Ce3+Ion is active ions.
A kind of preparation method of cerium dopping lutetium pyrosilicate scintillating ceramic, comprising the following steps:
A is by Lu2O3Powder, SiO2Powder, Ce2O3Powder is according to general formula (Lu0.94Ce0.06)2Si2O7In ion molar ratio example it is mixed
It closes uniformly, then the briquet under 180MPa pressure puts block into horse kettle furnace, 10h is sintered at 1200 DEG C into polycrystalline
LPS crystal, then polycrystalline LPS crystal is dosed into iridium crucible, in pure nitrogen gas or argon atmosphere, crystal is subjected to lifting life
Long, the revolving speed of crystal is 10r/min during lifting, and the speed-raising of crystal is 0.3mm/h, monocrystalline LPS crystal is obtained, by monocrystalline
LPS crystal pulverizes and sieves, and obtains LPS:Ce powder, and LPS:Ce powder and ethyl alcohol are mixed according to the volume ratio of 1:1, obtain mixing slurry
Material, carries out ball milling for mixed slurry；
B. the slurry after ball milling is crossed into 200 ~ 300 meshes, is then injected into mold and carries out moulding, then the air at 400 DEG C
Or it is calcined under oxygen atmosphere；
C. preliminary sintering: first carrying out dry-pressing for the LPS:Ce powder obtained after calcining, and the pressure of dry-pressing is 18MPa, after again to warp
The LPS:Ce for crossing dry-pressing carries out isostatic cool pressing, and the pressure of isostatic cool pressing obtains LPS:Ce just base, is tentatively sintered after being 100MPa
Temperature is 1300 DEG C, and preliminary sintering uses argon atmosphere, sintering time 3h.
D. double sintering: the pressure of argon gas is 50MPa in 350 DEG C of temperature-rise periods below;350 to 800 DEG C of heating
In the process, heating rate is 11 DEG C/min, and into 800 DEG C or more of temperature-rise periods, heating rate is 6 DEG C/min, until in furnace
Temperature reaches 2000 DEG C, after stopping 3h under the conditions of this temperature and pressure, 50 DEG C is cooled to the furnace, in 350 DEG C or more of heating
The pressure of gas gradually increases in the process, and pressure is advanced the speed as 40MPa/h；
E. annealing process: control heating rate is 5 DEG C/min, temperature is increased to 1200 DEG C, anneal 4h in air atmosphere.
Embodiment 3
A kind of cerium dopping lutetium pyrosilicate scintillating ceramic, the composition general formula of cerium dopping lutetium pyrosilicate scintillating ceramic are (Lu0.99Ce0.01)2Si2O7, Ce3+Ion is active ions.
A kind of preparation method of cerium dopping lutetium pyrosilicate scintillating ceramic, comprising the following steps:
A is by Lu2O3Powder, SiO2Powder, Ce2O3Powder is according to general formula (Lu0.99Ce0.01)2Si2O7In ion molar ratio example it is mixed
It closes uniformly, then the briquet under 190MPa pressure puts block into horse kettle furnace, 11h is sintered at 1100 DEG C into polycrystalline
LPS crystal, then polycrystalline LPS crystal is dosed into iridium crucible, in pure nitrogen gas or argon atmosphere, crystal is subjected to lifting life
Long, the revolving speed of crystal is 15r/min during lifting, and the speed-raising of crystal is 0.1mm/h, monocrystalline LPS crystal is obtained, by monocrystalline LPS
Crystal pulverizes and sieves, and obtains LPS:Ce powder.
B. the slurry after ball milling will be crossed 200 ~ 300 meshes, is then injected into mold and carries out moulding, then at 500 DEG C
Air or oxygen atmosphere under calcined；
C. preliminary sintering: first carrying out dry-pressing to LPS:Ce powder after calcining, and the pressure of dry-pressing is 19MPa, after again to passing through dry-pressing
LPS:Ce carry out isostatic cool pressing, the pressure of isostatic cool pressing obtains LPS:Ce after being 150MPa just base, the temperature being tentatively sintered are
1500 DEG C, preliminary sintering uses argon atmosphere, and sintering time 3h obtains LPS:Ce just base；By base at the beginning of LPS:Ce in argon gas gas
It is sintered under atmosphere；
D. double sintering: the pressure of argon gas is 45MPa in 350 DEG C of temperature-rise periods below;350 to 800 DEG C of temperature-rise period
In, heating rate is 10 DEG C/min, and into 800 DEG C or more of temperature-rise periods, heating rate is 5 DEG C/min, until in-furnace temperature
1950 DEG C are reached, after stopping 2.5h under the conditions of this temperature and pressure, 50 DEG C are cooled to the furnace, in 350 DEG C or more of heating
The pressure of gas gradually increases in journey, and pressure is advanced the speed as 35MPa/h；
E. annealing process: control heating rate is 10 DEG C/min, temperature is increased to 1250 DEG C, anneal 4h in air atmosphere.
Embodiment 4
The composition general formula of a kind of cerium dopping lutetium pyrosilicate scintillating ceramic, cerium dopping lutetium pyrosilicate scintillating ceramic is
(Lu0.999Ce0.001)2Si2O7, Ce3+Ion is active ions.
A kind of preparation method of cerium dopping lutetium pyrosilicate scintillating ceramic, comprising the following steps:
A is by Lu2O3Powder, SiO2Powder, Ce2O3Powder is according to general formula (Lu0.999Ce0.001)2Si2O7In ion molar ratio example it is mixed
It closes uniformly, then the briquet under 190MPa pressure puts block into horse kettle furnace, 11h is sintered at 1100 DEG C into polycrystalline
LPS crystal, then polycrystalline LPS crystal is dosed into iridium crucible, in pure nitrogen gas or argon atmosphere, crystal is subjected to lifting life
Long, the revolving speed of crystal is 15r/min during lifting, and the speed-raising of crystal is 0.1mm/h, monocrystalline LPS crystal is obtained, by monocrystalline LPS
Crystal pulverizes and sieves, and obtains LPS:Ce powder.
B. the slurry after ball milling will be crossed 200 ~ 300 meshes, is then injected into mold and carries out moulding, then at 500 DEG C
Air or oxygen atmosphere under calcined；
C. preliminary sintering: first carrying out dry-pressing to LPS:Ce powder after calcining, and the pressure of dry-pressing is 19MPa, after again to passing through dry-pressing
LPS:Ce carry out isostatic cool pressing, the pressure of isostatic cool pressing obtains LPS:Ce after being 150MPa just base, the temperature being tentatively sintered are
1500 DEG C, preliminary sintering uses argon atmosphere, and sintering time 3h obtains LPS:Ce just base；By base at the beginning of LPS:Ce in argon gas gas
It is sintered under atmosphere；
D. double sintering: the pressure of argon gas is 45MPa in 350 DEG C of temperature-rise periods below;350 to 800 DEG C of temperature-rise period
In, heating rate is 10 DEG C/min, and into 800 DEG C or more of temperature-rise periods, heating rate is 5 DEG C/min, until in-furnace temperature
1950 DEG C are reached, after stopping 2.5h under the conditions of this temperature and pressure, 50 DEG C are cooled to the furnace, in 350 DEG C or more of heating
The pressure of gas gradually increases in journey, and pressure is advanced the speed as 30MPa/h；
E. annealing process: control heating rate is 10 DEG C/min, temperature is increased to 1250 DEG C, anneal 4h in air atmosphere.
Embodiment 5
A kind of cerium dopping lutetium pyrosilicate scintillating ceramic, the composition general formula of cerium dopping lutetium pyrosilicate scintillating ceramic are (Lu0.98Ce0.02)2Si2O7, Ce3+Ion is active ions.
A kind of preparation method of cerium dopping lutetium pyrosilicate scintillating ceramic, comprising the following steps:
A is by Lu2O3Powder, SiO2Powder, Ce2O3Powder is according to general formula (Lu0.99Ce0.01)2Si2O7In ion molar ratio example it is mixed
It closes uniformly, then the briquet under 190MPa pressure puts block into horse kettle furnace, 11h is sintered at 1100 DEG C into polycrystalline
LPS crystal, then polycrystalline LPS crystal is dosed into iridium crucible, in pure nitrogen gas or argon atmosphere, crystal is subjected to lifting life
Long, the revolving speed of crystal is 15r/min during lifting, and the speed-raising of crystal is 0.1mm/h, monocrystalline LPS crystal is obtained, by monocrystalline LPS
Crystal pulverizes and sieves, and obtains LPS:Ce powder.
B. the slurry after ball milling will be crossed 200 meshes, is then injected into mold and carries out moulding, then the sky at 500 DEG C
It is calcined under gas or oxygen atmosphere；
C. preliminary sintering: first carrying out dry-pressing to LPS:Ce powder after calcining, and the pressure of dry-pressing is 19MPa, after again to passing through dry-pressing
LPS:Ce carry out isostatic cool pressing, the pressure of isostatic cool pressing obtains LPS:Ce after being 150MPa just base, the temperature being tentatively sintered are
1500 DEG C, preliminary sintering uses argon atmosphere, and sintering time 3h obtains LPS:Ce just base；By base at the beginning of LPS:Ce in argon gas gas
It is sintered under atmosphere；
D. double sintering: the pressure of argon gas is 45MPa in 350 DEG C of temperature-rise periods below;350 to 800 DEG C of temperature-rise period
In, heating rate is 10 DEG C/min, and into 800 DEG C or more of temperature-rise periods, heating rate is 5 DEG C/min, until in-furnace temperature
1950 DEG C are reached, after stopping 2.5h under the conditions of this temperature and pressure, 50 DEG C are cooled to the furnace, in 350 DEG C or more of heating
The pressure of gas gradually increases in journey, and pressure is advanced the speed as 32MPa/h；
E. annealing process: control heating rate is 10 DEG C/min, temperature is increased to 1250 DEG C, anneal 4h in air atmosphere.
Translucent staring optical ceramics are obtained after each finely ground polishing of embodiment of the present invention, relative density is all larger than
99%.Good luminescent properties are shown under the conditions of burst of ultraviolel, luminous intensity reaches the 65% of Ce:Lu2SiO5 monocrystalline
More than.
Claims (9)
1. a kind of cerium dopping lutetium pyrosilicate scintillating ceramic, it is characterised in that: the group of the cerium dopping lutetium pyrosilicate scintillating ceramic
It is (Lu at general formula1-xCex)2Si2O7, wherein x=0.001-0.06.
2. a kind of cerium dopping lutetium pyrosilicate scintillating ceramic according to claim 1, it is characterised in that: the general formula
(Lu1-xCex)2Si2O7In Ce3+Ion is active ions.
3. a kind of preparation method of cerium dopping lutetium pyrosilicate scintillating ceramic according to claim 1, which is characterized in that including
Following steps:
A is (Lu according to chemical formula1-xCex)2Si2O7Proportion preparation LPS:Ce powder, by LPS:Ce powder and ethyl alcohol according to 1:(1~
4) volume ratio mixing, obtains mixed slurry, mixed slurry is carried out ball milling；
B. 200 ~ 300 meshes will be crossed after the slurry ball milling after ball milling, be then injected into mold and carry out moulding, then in 400-1000
It is calcined under air or oxygen atmosphere at DEG C；
C. preliminary sintering: base at the beginning of the LPS:Ce powder obtained after calcining obtains LPS:Ce after pressure forming；By base at the beginning of LPS:Ce
It is sintered under an argon atmosphere；
D. it double sintering: will be sintered again under an argon atmosphere by the first base being tentatively sintered；
E. annealing process: control heating rate is 5-20 DEG C/min, temperature is increased to 1200-1300 DEG C, in air atmosphere
Anneal 4-10h, obtains cerium dopping lutetium pyrosilicate scintillating ceramic.
4. a kind of preparation method of cerium dopping lutetium pyrosilicate scintillating ceramic according to claim 3, it is characterised in that: described
LPS:Ce powder using following steps prepare: by Lu2O3Powder, SiO2Powder, Ce2O3Powder is according to general formula (Lu1-xCex)2Si2O7In ion molar ratio example be uniformly mixed, then the briquet under 180-200MPa pressure puts block into horse kettle furnace
In, it is sintered 10-12h at 1200-1300 DEG C into polycrystalline LPS crystal, the polycrystalline LPS crystal is pulverized and sieved, LPS is obtained:
Ce powder.
5. a kind of preparation method of cerium dopping lutetium pyrosilicate scintillating ceramic according to claim 3, it is characterised in that: described
LPS:Ce powder using following steps prepare: by Lu2O3Powder, SiO2Powder, Ce2O3Powder is according to general formula (Lu1-xCex)2Si2O7In ion molar ratio example be uniformly mixed, then the briquet under 180-200MPa pressure puts block into horse kettle furnace
In, 10-12h is sintered at 1200-1300 DEG C and is dosed into iridium crucible at polycrystalline LPS crystal, then by polycrystalline LPS crystal, pure
In nitrogen or argon atmosphere, crystal carries out pulling growth, obtains monocrystalline LPS crystal, the monocrystalline LPS crystal is pulverized and sieved,
Obtain LPS:Ce powder.
6. a kind of preparation method of cerium dopping lutetium pyrosilicate scintillating ceramic according to claim 5, it is characterised in that: in institute
The revolving speed of crystal is 10-20r/min during the lifting stated, and the speed-raising of crystal is 0.2-0.3mm/h.
7. a kind of preparation method of cerium dopping lutetium pyrosilicate scintillating ceramic according to claim 3, it is characterised in that: first right
LPS:Ce powder carries out dry-pressing, and the pressure of the dry-pressing is 18-20MPa, after it is cold to the LPS:Ce progress Jing Guo dry-pressing etc. again
Static pressure, the pressure of the isostatic cool pressing obtains LPS:Ce after being 100-200MPa just base, the temperature being tentatively sintered are
1300 DEG C -2000 DEG C, the preliminary sintering uses argon atmosphere, sintering time 3-4h.
8. a kind of preparation method of cerium dopping lutetium pyrosilicate scintillating ceramic according to claim 3, it is characterised in that: in institute
During the double sintering stated, the pressure of argon gas is 40-50MPa in 350 DEG C of temperature-rise periods below;350 to 800 DEG C of liter
During temperature, heating rate is 10-11 DEG C/min, and into 800 DEG C or more of temperature-rise periods, heating rate is 5-6 DEG C/min, directly
1900-2000 DEG C is reached to in-furnace temperature, after stopping 2-3h under the conditions of this temperature and pressure, cools to 50 ~ 60 DEG C with the furnace.
9. a kind of preparation method of cerium dopping lutetium pyrosilicate scintillating ceramic according to claim 8, it is characterised in that:
The pressure of gas gradually increases in 350 DEG C or more of temperature-rise period, and the pressure is advanced the speed as 30-40MPa/h.
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| CN110128120A (en) * | 2019-05-10 | 2019-08-16 | 福建省长汀金龙稀土有限公司 | A kind of preparation method of composite ceramics |
| CN110734223A (en) * | 2019-11-21 | 2020-01-31 | 北方工业大学 | lutetium-doped silicate scintillation glass and preparation method thereof |
| 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 |
| CN112573905A (en) * | 2020-12-24 | 2021-03-30 | 中国科学院上海硅酸盐研究所 | Anion-doped garnet scintillator and preparation method and application thereof |
| CN114195656A (en) * | 2021-11-29 | 2022-03-18 | 华南理工大学 | Large-area high-transmittance metal halide scintillating ceramic and preparation method thereof |
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| CN107555977A (en) * | 2017-07-14 | 2018-01-09 | 上海大学 | Cerium dopping silicic acid lutetium scintillating ceramic and its HIP sintering preparation method |
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| CN110128120A (en) * | 2019-05-10 | 2019-08-16 | 福建省长汀金龙稀土有限公司 | A kind of preparation method of composite ceramics |
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| CN110734223A (en) * | 2019-11-21 | 2020-01-31 | 北方工业大学 | lutetium-doped silicate scintillation glass and preparation method thereof |
| CN110734223B (en) * | 2019-11-21 | 2022-03-08 | 北方工业大学 | Lutetium-doped silicate scintillation glass and preparation method thereof |
| 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 |
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| CN112573905A (en) * | 2020-12-24 | 2021-03-30 | 中国科学院上海硅酸盐研究所 | Anion-doped garnet scintillator and preparation method and application thereof |
| CN114195656A (en) * | 2021-11-29 | 2022-03-18 | 华南理工大学 | Large-area high-transmittance metal halide scintillating ceramic and preparation method thereof |
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