CN110256073A - Ce:GAGG fluorescence ceramics and its preparation preparation method, preparation system - Google Patents
Ce:GAGG fluorescence ceramics and its preparation preparation method, preparation system Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000000126 substance Substances 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 14
- 238000000137 annealing Methods 0.000 claims description 13
- 238000010792 warming Methods 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 235000015895 biscuits Nutrition 0.000 claims description 10
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 10
- 229910052593 corundum Inorganic materials 0.000 claims description 10
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 210000001161 mammalian embryo Anatomy 0.000 claims description 8
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 7
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 description 6
- 238000003825 pressing Methods 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000009461 vacuum packaging Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 230000005251 gamma ray Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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Abstract
The present invention provides a kind of Ce:GAGG fluorescence ceramics and preparation method thereof and preparation system, uses Gd3+Replace Y completely3+,Ga3+Replace Al3+The chemical formula Gd of formation3‑xAl5‑yGayO12:Cex, by controlling Ce3+Ion, Ga3+The concentration of ion adjusts Ga3+Ion and Ce3+Energy transfer between ion realizes the high delivery efficiency of Ce:GAGG fluorescence ceramics.
Description
Technical field
The present invention relates to solid-state lighting field of material technology, especially a kind of Ce:GAGG fluorescence ceramics and preparation method thereof,
Preparation system.
Background technique
Background that this section is intended to provide an explanation of the embodiments of the present invention set forth in the claims or context.Herein
Description recognizes it is the prior art not because not being included in this section.
The ionising radiation of high-energy is converted to thousands of optical photon by Inorganic scintillation physical efficiency, in many radiation detections
Field plays always important function, including medical image, and safety, astrophysics and geophysics and resource are explored.At this
In a little applications, application of the scintillator on γ-ray detector has attracted the concern in terms of medical treatment and security application.To mesh
Before until, most of scintillation detectors are made of monocrystalline, mainly due to their high optical quality.
However Ce:YAG fluorescent transparent ceramics, light output (LY) are higher than monocrystalline, this is mainly due to be included in forbidden band
The antisite defect for capturing electronics again on anti position level is inhibited, and antisite defect will lead to lower light output effect
Rate.And the light output of Ce:GAGG fluorescence ceramics reaches 46000ph/Mev, therefore prepares height using upper in γ-ray detector
The Ce:GAGG fluorescence ceramics of delivery efficiency are of great significance.
Summary of the invention
In view of the foregoing, it is necessary to a kind of Ce:GAGG fluorescence ceramics and preparation method thereof and preparation system are provided, it can
To prepare the fluorescence ceramics piece of high delivery efficiency.
A kind of technical solution provided by the invention are as follows: preparation method of Ce:GAGG fluorescence ceramics, comprising the following steps:
Step 1: by Gd2O3、Al2O3、CeO2、Ga2O3Raw material is uniformly mixed after weighing by chemical formula proportion, is put into stainless steel
In mold, mixed powder is pressed into idiosome under the certain pressure time；
Step 2: idiosome is further pressed into fine and close plain embryo under the certain pressure time；
Step 3: plain embryo being sintered, fluorescence ceramics piece sample is obtained；
Step 4: gained sample being made annealing treatment, obtaining chemical formula is Gd3-xAl5-yGayO12:CexFluorescence ceramics,
Wherein Ce3+Concentration x be 0.001~0.06, Ga3+Concentration y be 0~4.
Further, the size of stainless steel mould is 20~100mm of diameter, 20~80mm of depth in step 1.
Further, pressure is 3~20t in step 1, and the dwell time is 5~20min.
Further, pressure is 50~300MPa in step 2.
Further, the dwell time is 5~20min in step 2.
Further, sintering condition in step 3: 1200~1600 DEG C are warming up to the rate of 1~10 DEG C/min, heat preservation 2
~20h, vacuum degree 10-4~10-3Pa。
Further, condition is made annealing treatment in step 4: being warming up to 1200~1500 DEG C with the rate of 6~10 DEG C/min, protect
5~10h of temperature.
The present invention separately provides a kind of Ce:GAGG fluorescence ceramics, is obtained by the preparation method of above-mentioned Ce:GAGG fluorescence ceramics
It arrives, the fluorescence ceramics have high delivery efficiency.
The present invention provides a kind of preparation system of Ce:GAGG fluorescence ceramics again, and the preparation system includes weighing equipment, mixes
Material machine, hydraulic press, cold isostatic press, vacuum sintering furnace and high temperature resistance furnace, wherein
Weighing equipment is used for Gd2O3、Al2O3、CeO2、Ga2O3Raw material weighing；
Batch mixer, it is uniformly mixed for carrying out various raw materials；
Green body is made for mixed powder to be kept 5~20min duration under 3~20t pressure in hydraulic press；
Fine and close element is made for green body to be kept 5~20min duration under 50~300MPa pressure in cold isostatic press
Base；
Vacuum sintering furnace controls its vacuum degree 10-4~10-3Pa, heating rate is 1~10 DEG C/min, for biscuit to exist
2~20h is kept the temperature at a temperature of 1200~1600 DEG C, sintering obtains fluorescence ceramics piece sample；
High temperature resistance furnace, controlling its heating rate is 6~10 DEG C/min, for by fluorescence ceramics piece sample 1200~
5~10h is kept the temperature at a temperature of 1500 DEG C, it is Gd that annealing, which obtains chemical formula,3-xAl5-yGayO12:CexFluorescence ceramics, wherein Ce3 +Concentration x be 0.001~0.06, Ga3+Concentration y be 0~4.
Further, the chemical formula is Gd3-xAl5-yGayO12: the quantum efficiency of the fluorescence ceramics of Cex reaches 80%~
90%.
Compared with prior art, Ce:GAGG fluorescence ceramics preparation method provided by the invention, comprising the following steps: will
Gd2O3, Al2O3, CeO2, Ga2O3 raw material are uniformly mixed after weighing by chemical formula proportion, by mixed powder under the certain pressure time
Material is pressed into idiosome；Idiosome is further pressed into fine and close plain embryo under the certain pressure time；Plain embryo is sintered, is obtained
Fluorescence ceramics piece sample；Gained sample is made annealing treatment, obtaining chemical formula is Gd3-xAl5-yGayO12:CexFluorescence pottery
Porcelain, wherein Ce3+Concentration x be 0.001~0.06, Ga3+Concentration y be 0~4.The present invention is by using Gd3+Replace Y completely3+,
Ga3+Replace Al3+The chemical formula Gd of formation3-xAl5-yGayO12:Cex, by controlling Ce3+Ion, Ga3+The concentration of ion adjusts Ga3+
Ion and Ce3+Energy transfer between ion realizes the high delivery efficiency of Ce:GAGG fluorescence ceramics.
Detailed description of the invention
Fig. 1 is the Ce:GAGG fluorescence ceramics piece prepared in an embodiment of the present invention and pair of GAGG single crystal luminescent intensity
Than figure.
Fig. 2 is the preparation system schematic diagram of Ce:GAGG fluorescence ceramics in an embodiment of the present invention.
Description of symbols:
| Weighing equipment | 101 |
| Batch mixer | 103 |
| Hydraulic press | 105 |
| Cold isostatic press | 107 |
| Vacuum sintering furnace | 109 |
| High temperature resistance furnace | 111 |
The present invention that the following detailed description will be further explained with reference to the above drawings.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
It should be noted that it can be directly on another component when component is referred to as " being installed in " another component
Or there may also be components placed in the middle.When a component is considered as " being set to " another component, it, which can be, is directly set
Set on another component or may be simultaneously present component placed in the middle.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein " and/or " it include one or more phases
Any and all combinations of the listed item of pass.
Referring to Fig. 1, Fig. 2, a kind of preparation method of Ce:GAGG fluorescence ceramics, comprising the following steps:
Step 1: by Gd2O3、Al2O3、CeO2、Ga2O3Raw material is uniformly mixed after weighing by chemical formula proportion, is put into stainless steel
In mold, mixed powder is pressed into idiosome under the certain pressure time；
Step 2: idiosome is further pressed into fine and close plain embryo under the certain pressure time；
Step 3: plain embryo being sintered, fluorescence ceramics piece sample is obtained；
Step 4: gained sample being made annealing treatment, obtaining chemical formula is Gd3-xAl5-yGayO12:CexFluorescence ceramics,
Wherein Ce3+Concentration x be 0.001~0.06, Ga3+Concentration y be 0~4.
In the present embodiment, the size of stainless steel mould is 20~100mm of diameter, 20~80mm of depth, pressure in step 1
Pressing pressure is 3~20t, and the dwell time is 5~20min；Pressure is 50~300MPa in step 2, and the dwell time is 5~20min.
In the present embodiment, sintering condition is that the rate of 1~10 DEG C/min is warming up to 1200~1600 DEG C in step 3,
Keep the temperature 2~20h, vacuum degree 10-4~10-3Pa。
In the present embodiment, condition is made annealing treatment in step 4: 1200 are warming up to the rate of 6~10 DEG C/min~
1500 DEG C, keep the temperature 5~10h.
It as described in Figure 2, is the preparation system schematic diagram of Ce:GAGG fluorescence ceramics in an embodiment of the present invention.The system
Standby system includes weighing equipment, batch mixer, hydraulic press, cold isostatic press, vacuum sintering furnace and high temperature resistance furnace, wherein
Weighing equipment is used for Gd2O3、Al2O3、CeO2、Ga2O3Raw material weighing；
Batch mixer, it is uniformly mixed for carrying out various raw materials；
Green body is made for mixed powder to be kept 5~20min duration under 3~20t pressure in hydraulic press；
Fine and close element is made for green body to be kept 5~20min duration under 50~300MPa pressure in cold isostatic press
Base；
Vacuum sintering furnace controls its vacuum degree 10-4~10-3Pa, heating rate is 1~10 DEG C/min, for biscuit to exist
2~20h is kept the temperature at a temperature of 1200~1600 DEG C, sintering obtains fluorescence ceramics piece sample；
High temperature resistance furnace, controlling its heating rate is 6~10 DEG C/min, for by fluorescence ceramics piece sample 1200~
5~10h is kept the temperature at a temperature of 1500 DEG C, it is Gd that annealing, which obtains chemical formula,3-xAl5-yGayO12: the fluorescence ceramics of Cex, wherein
Ce3+Concentration x be 0.001~0.06, Ga3+Concentration y be 0~4.
Embodiment 1
By Gd2.97Al4.95Ga0.05O12:Ce0.03, stoichiometric ratio weighs Gd respectively2O35.383g、Al2O32.524g、
Ga2O30.047g、CeO20.0516g, which is added in ball grinder, obtains mixture in 3 hours with 400r/min revolving speed ball milling, then will
Mixture is put into diameter 30mm, in the stainless steel mould of depth 60mm, green body is obtained with 10t pressure dry-pressing 10min, then by base
It is that pressure maintaining 5min obtains biscuit in 300MPa cold isostatic press, then biscuit is burnt in vacuum that body, which is put into vacuum packaging bag in pressure,
1550 DEG C are warming up to 3 DEG C/min in freezing of a furnace, keeps the temperature 5 hours, vacuum degree is 8 × 10-4, then 1400 are warming up to 6 DEG C/min
It DEG C is made annealing treatment, keeps the temperature 6 hours, ceramic sheet is finally carried out cutting and polishing processing by furnace cooling, and thickness is made
0.15cm fluorescent transparent ceramics.Referring to Fig. 1, Fig. 1 is GAGG potsherd made from the present embodiment and GAGG single crystal luminescent intensity
Comparison diagram, it can be seen that the luminous intensity of GAGG potsherd is apparently higher than GAGG single crystal luminescent intensity, and in the hair of 540nm
Luminous intensity is 2~3 times of monocrystalline.
Embodiment 2
By Gd2.94Al4.92Ga0.08O12:Ce0.06, stoichiometric ratio weighs Gd respectively2O35.328g、Al2O32.508g、
Ga2O30.075g、CeO20.103g, which is added in ball grinder, obtains mixture in 3 hours with 400r/min revolving speed ball milling, then will mix
It closes object and is put into diameter 30mm, in the stainless steel mould of depth 60mm, green body is obtained with 10t pressure dry-pressing 10min, then by green body
It is put into vacuum packaging bag and obtains biscuit in pressure for pressure maintaining 5min in 250MPa cold isostatic press, then by biscuit in vacuum-sintering
1450 DEG C are warming up to 4 DEG C/min in furnace, keeps the temperature 6 hours, vacuum degree is 8 × 10-4, then 1500 DEG C are warming up to 8 DEG C/min
It is made annealing treatment, keeps the temperature 6 hours, ceramic sheet is finally carried out cutting and polishing processing by furnace cooling, and thickness 0.20cm is made
Fluorescent transparent ceramics.
Embodiment 3
By Gd2.98Al4.97Ga0.03O12:Ce0.02, stoichiometric ratio weighs Gd respectively2O35.401g、Al2O32.534g、
Ga2O30.028g、CeO20.034g, which is added in ball grinder, obtains mixture in 3 hours with 400r/min revolving speed ball milling, then will mix
It closes object and is put into diameter 30mm, in the stainless steel mould of depth 60mm, green body is obtained with 10t pressure dry-pressing 10min, then by green body
It is put into vacuum packaging bag and obtains biscuit in pressure for pressure maintaining 5min in 250MPa cold isostatic press, then by biscuit in vacuum-sintering
1600 DEG C are warming up to 5 DEG C/min in furnace, keeps the temperature 4 hours, vacuum degree is 8 × 10-4, then 1300 DEG C are warming up to 8 DEG C/min
It is made annealing treatment, keeps the temperature 6 hours, ceramic sheet is finally carried out cutting and polishing processing by furnace cooling, and thickness 0.15cm is made
Fluorescent transparent ceramics.
Embodiment of above is only to illustrate the technical solution of the embodiment of the present invention rather than limits, although referring to above preferable
The embodiment of the present invention is described in detail in embodiment, those skilled in the art should understand that, it can be to this hair
The technical solution of bright embodiment is modified or equivalent replacement should not all be detached from the embodiment of the present invention technical solution spirit and
Range.
Claims (10)
1. a kind of preparation method of Ce:GAGG fluorescence ceramics, which comprises the following steps:
Step 1: by Gd2O3、Al2O3、CeO2、Ga2O3Raw material is uniformly mixed after weighing by chemical formula proportion, is put into stainless steel mould
In, mixed powder is pressed into idiosome under the certain pressure time；
Step 2: idiosome is further pressed into fine and close plain embryo under the certain pressure time；
Step 3: plain embryo being sintered, fluorescence ceramics piece sample is obtained；
Step 4: gained sample being made annealing treatment, obtaining chemical formula is Gd3-xAl5-yGayO12:CexFluorescence ceramics, wherein
Ce3+Concentration x be 0.001~0.06, Ga3+Concentration y be 0~4.
2. the preparation method of Ce:GAGG fluorescence ceramics as described in claim 1, it is characterised in that: stainless steel mould in step 1
Size be 20~100mm of diameter, 20~80mm of depth.
3. the preparation method of Ce:GAGG fluorescence ceramics as described in claim 1, it is characterised in that: in step 1 pressure be 3~
20t, dwell time are 5~20min.
4. the preparation method of Ce:GAGG fluorescence ceramics as described in claim 1, it is characterised in that: in step 2 pressure be 50~
300MPa。
5. the preparation method of Ce:GAGG fluorescence ceramics as described in claim 1, it is characterised in that: the dwell time is in step 2
5~20min.
6. the preparation method of Ce:GAGG fluorescence ceramics as described in claim 1, it is characterised in that: sintering condition in step 3:
1200~1600 DEG C are warming up to the rate of 1~10 DEG C/min, keeps the temperature 2~20h, vacuum degree 10-4~10-3Pa。
7. the preparation method of Ce:GAGG fluorescence ceramics as described in claim 1, it is characterised in that: make annealing treatment item in step 4
Part: 1200~1500 DEG C are warming up to the rate of 6~10 DEG C/min, keeps the temperature 5~10h.
8. a kind of Ce:GAGG fluorescence ceramics, it is characterised in that: glimmering by Ce:GAGG such as of any of claims 1-7
The preparation method of light ceramic obtains, and the fluorescence ceramics have high delivery efficiency.
9. a kind of preparation system of Ce:GAGG fluorescence ceramics, it is characterised in that: the preparation system includes weighing equipment, mixing
Machine, hydraulic press, cold isostatic press, vacuum sintering furnace and high temperature resistance furnace, wherein
Weighing equipment is used for Gd2O3、Al2O3、CeO2、Ga2O3Raw material weighing；
Batch mixer, it is uniformly mixed for carrying out various raw materials；
Green body is made for mixed powder to be kept 5~20min duration under 3~20t pressure in hydraulic press；
Fine and close biscuit is made for green body to be kept 5~20min duration under 50~300MPa pressure in cold isostatic press；
Vacuum sintering furnace controls its vacuum degree 10-4~10-3Pa, heating rate are 1~10 DEG C/min, are used for biscuit 1200
2~20h is kept the temperature at a temperature of~1600 DEG C, sintering obtains fluorescence ceramics piece sample；
High temperature resistance furnace, controlling its heating rate is 6~10 DEG C/min, is used for fluorescence ceramics piece sample at 1200~1500 DEG C
At a temperature of keep the temperature 5~10h, annealing obtain chemical formula be Gd3-xAl5-yGayO12: the fluorescence ceramics of Cex, wherein Ce3+It is dense
Degree x is 0.001~0.06, Ga3+Concentration y be 0~4.
10. the preparation system of Ce:GAGG fluorescence ceramics as claimed in claim 9, it is characterised in that: the chemical formula is Gd3- xAl5-yGayO12: the quantum efficiency of the fluorescence ceramics of Cex reaches 80%~90%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110746970A (en) * | 2019-11-19 | 2020-02-04 | 吉安县惠鑫实业有限责任公司 | Ga3+/Ce3+Codoped GdAG multicolor fluorescent powder |
| CN115650725A (en) * | 2022-10-12 | 2023-01-31 | 中国科学院上海光学精密机械研究所 | Fluorescent ceramic material with multiband fluorescent emission and preparation method thereof |
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