CN116496788B - Method for enhancing luminous intensity of terbium-doped gadolinium oxysulfide fluorescent material - Google Patents
Method for enhancing luminous intensity of terbium-doped gadolinium oxysulfide fluorescent material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 24
- 230000002708 enhancing effect Effects 0.000 title abstract description 4
- MCVAAHQLXUXWLC-UHFFFAOYSA-N [O-2].[O-2].[S-2].[Gd+3].[Gd+3] Chemical compound [O-2].[O-2].[S-2].[Gd+3].[Gd+3] MCVAAHQLXUXWLC-UHFFFAOYSA-N 0.000 title description 2
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 238000004020 luminiscence type Methods 0.000 claims abstract description 11
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 230000005284 excitation Effects 0.000 claims description 9
- 238000000295 emission spectrum Methods 0.000 claims description 8
- 238000000695 excitation spectrum Methods 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 abstract description 4
- 230000003595 spectral effect Effects 0.000 abstract 1
- 238000005424 photoluminescence Methods 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 238000010532 solid phase synthesis reaction Methods 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000003384 imaging method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- -1 rare earth nitrate Chemical class 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 230000018199 S phase Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 241001199012 Usta Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000005136 cathodoluminescence Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002059 diagnostic imaging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 1
- 238000002284 excitation--emission spectrum Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000001748 luminescence spectrum Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000004297 night vision Effects 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 239000012856 weighed raw material Substances 0.000 description 1
- 238000004875 x-ray luminescence Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7767—Chalcogenides
- C09K11/7769—Oxides
- C09K11/7771—Oxysulfides
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- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a method for enhancing Gd 2 O 2 S:Tb 3+ Method for exciting and emitting spectral intensity by using Gd as raw material 2 (SO 4 ) 3 ·8H 2 O、Gd 2 O 3 Powder C and Tb 4 O 7 And sintering aids KCl, liF and K 3 PO 4 ·3H 2 O is weighed according to the stoichiometric ratio and ground to be uniformly mixed, and calcined for 0.5 to 6 hours at the temperature of 1150 to 1450 ℃ by using a double-carbon reduction technology, thus obtaining the Gd with excellent luminescence performance 2 O 2 S:Tb 3+ Fluorescent material powder.
Description
Technical Field
The invention relates to a method for enhancing Gd 2 O 2 S:Tb 3+ The method adopts a double-carbon reduction technology, and can prepare Gd with excellent luminous performance in one step by selecting and adjusting the proportion of the fluxing agent 2 O 2 S:Tb 3+ Fluorescent material Gd 2 O 2 S:Tb 3+ The excitation and emission spectrum intensity of the fluorescent material is effectively improved, and the technology belongs to the field of photoelectric functional materials.
Background
Gd is currently used in image intensifier and X-ray detection and imaging techniques 2 O 2 S:Tb 3+ The fluorescent screen prepared from the luminescent materials is a key device of an image intensifier and a scintillator detector, and is an important component for realizing the functions of cathode ray luminescence and X-ray luminescence. Wherein Gd is 2 O 2 S:Tb 3+ Compared with other luminescent materials, the Gd luminescent material has the advantages of high imaging speed, stable performance and lower cost, so Gd luminescent material with excellent luminescent performance is developed 2 O 2 S:Tb 3+ The fluorescent material has remarkable research value and important research significance for improving the performance of an image intensifier, realizing low-dose X-ray medical imaging and the like.
Gd 2 O 2 S:Tb 3+ The fluorescent material is a rare earth doped oxysulfide-based fluorescent material, and the oxysulfide matrix has the characteristics of low phonon energy, stable chemical property and strong thermal stability compared with luminescent material matrixes such as fluoride, oxide, halide and the like. Wherein Gd is 2 O 2 S has a wider forbidden bandwidth (4.6-4.8 eV), is an excellent luminescent material matrix, and has good light absorption and transmission capability. Current preparation of Gd 2 O 2 S:Tb 3+ Mainly comprises a high-temperature solid-phase method, a hydrothermal method, a solvothermal method, a combustion method, a coprecipitation method and the like, and Song et al in 2010 obtain a precursor by heating the precursor in a stainless steel autoclave at 200 ℃ through a simple solvothermal method, and the precursor is prepared by adding an inert N 2 And carrying out heat treatment at 600-800 ℃ for 2 hours in the S atmosphere to obtain the final product. Successfully realizes good dispersion and uniform submicron spherical Gd 2 O 2 S:Tb 3+ Fluorescent material. In 2009 Xing et al, a monodispersed spherical Gd was successfully prepared by combining a modified homogeneous precipitation method with a solid-gas vulcanization technique 2 O 2 S:Tb 3+ Nanoparticles, the resulting samples exhibit excellent luminescence properties, compared to Gd prepared by a complex precipitation method 2 O 2 S:Tb 3+ The luminescent intensity of the nanoparticle is improved by about 50% at a lower sulfidation temperature. In 2013 Hernez-adam et al, thermal precipitation by aqueous ureaThe method comprises the steps of sintering and calcining, wherein the precipitate obtained by the urea aqueous thermal precipitation method of rare earth nitrate is subjected to heat treatment at 800 ℃ for 3 hours to obtain Gd 2 O 3 :Tb 3+ The precursor is annealed at 800 ℃ by a sulfur vapor method to successfully obtain nano Gd 2 O 2 S:Tb 3+ Fluorescent material. He et al in 2015 used a microwave solid phase method, heated at 900W for 10 minutes, then heated at 800W for 15 minutes, and repeatedly heated again to synthesize Gd 2 O 2 S:Tb 3+ The fluorescent material shows a strong green emission peak at 546nm under the excitation of ultraviolet rays and cathode rays, can obtain better luminescence performance compared with the traditional high-temperature solid phase method, and shows good luminescence stability. In 2020, usta baev et al added Na in the conventional high temperature solid phase method 2 CO 3 And S as raw material, na 2 CO 3 Polysulfide Na formed by reaction with S 2 S x Continue to react with Gd 2 O 3 The reaction generates Gd 2 O 2 S:Tb 3+ The method researches the influence of synthetic atmosphere, raw material mixture content and fluxing agent content on phase composition and luminous intensity. To obtain Gd without mixed phase 2 O 2 S:Tb 3 + And emits light under X-ray excitation. However, at present Gd 2 O 2 S:Tb 3+ Gd with better luminous efficiency and higher luminous intensity is still needed in the application of fluorescent material in realizing high-resolution and high-sensitivity X-ray imaging, low-light night vision and the like 2 O 2 S:Tb 3+ Development of fluorescent materials.
Disclosure of Invention
To improve Gd 2 O 2 S:Tb 3+ The invention provides a fluorescent material with enhanced luminescent property 2 O 2 S:Tb 3+ The preparation technology of fluorescence material excitation and emission spectrum intensity.
The invention is characterized in that Gd 2 O 2 S:Tb 3+ Gd is used in the preparation process of the fluorescent material 2 O 3 、Gd 2 (SO 4 ) 3 ·8H 2 O, C powder is used as raw material, adopts a double-carbon reduction technology, and is innovatively producedThe raw material selection and the addition mode of multiple fluxing agents combined enhanced luminescence optimize the process method, so that the Gd prepared by the process method 2 O 2 S:Tb 3+ The fluorescent material has more excellent luminescence property.
Gd is used in the process of selecting raw materials 2 (SO4) 3 ·8H 2 O is used as a sulfur source of sulfur oxide, gd 2 (SO 4 ) 3 ·8H 2 O and Gd 2 O 3 Co-composition of synthetic Gd 2 O 2 Gd of S 3+ And the source reduces the introduction of impurity ions. By KCl, liF and K 3 PO 4 The combination of various fluxing agents reduces the temperature required by the reaction, promotes the growth of crystal grains, reduces the impurity phase in the phase structure and promotes the doping of rare earth ions into a matrix lattice. Gd with excellent luminescence performance is generated by utilizing a double-carbon reduction technology in the calcination process of 0.5-6h at 1150-1450 DEG C 2 O 2 S:Tb 3+ Fluorescent material.
The invention provides sulfur source by rare earth sulfate and simultaneously is used for synthesizing Gd 2 O 2 Gd of S matrix 3+ One of the sources, no SO in the preparation process 2 The invention has two important meanings, namely, the Gd is enhanced 2 O 2 S:Tb 3+ The luminescent property of the fluorescent material, and secondly, provides a preparation technology which is synthesized in one step, has a simple process method and is environment-friendly.
Drawings
FIG. 1 is Gd of the invention 2 O 2 S:Tb 3+ XRD pattern of fluorescent material sample.
FIG. 2 is Gd of the invention 2 O 2 S:Tb 3+ Photoluminescence excitation spectrum of fluorescent material sample.
FIG. 3 is Gd of the invention 2 O 2 S:Tb 3+ Photoluminescence emission spectrum of a fluorescent material sample.
FIG. 4 is Gd of the invention 2 O 2 S:Tb 3+ SEM image of fluorescent material sample.
FIG. 5 is the presentGd of the invention 2 O 2 S:Tb 3+ Cathode ray luminescence spectrum of fluorescent material sample.
FIG. 6 is a graph of the different sintering aids Gd 2 O 2 S:Tb 3+ Photoluminescence emission spectrum of a fluorescent material sample.
FIG. 7 is a graph of the different sintering aids Gd 2 O 2 S:Tb 3+ Cathode ray excitation emission spectrum of fluorescent material sample.
Detailed Description
Gd of the present invention having excellent luminescence properties 2 O 2 S:Tb 3+ The specific process of the fluorescent material is described in detail as follows:
(1) By Gd 2 (SO 4 ) 3 ·8H 2 O，Gd 2 O 3 (A.R)，Tb 4 O 7 (A.R) and C powder (A.R) as raw materials, KCl (A.R), liF (A.R) and K are selected 3 PO 4 ·3H 2 O (A.R) is a sintering aid. According to Gd 2-x O 2 S:0.07Tb 3+ The stoichiometric ratio of each raw material was calculated. The content of sintering aid was 14wt%, 9wt% and 7wt% of the product, respectively;
(2) According to the preparation of 5g sample, a precise electronic balance is adopted to weigh the corresponding amount of Gd 2 (SO 4 ) 3 ·8H 2 O，Gd 2 O 3 ，Tb 4 O 7 Powder C, KCl, liF and K 3 PO 4 ·3H 2 O raw materials, namely, putting the weighed raw materials into an agate mortar, grinding for 20-60 min, uniformly mixing the raw materials, and putting the raw materials into an alumina crucible with the size of 25 ml;
(3) Selecting an alumina crucible with the size of 100ml, filling excessive C powder, sleeving a crucible with the size of 25ml containing raw materials into the crucible with the size of 100ml, and feeding into a box-type resistance furnace;
(4) Starting sintering, wherein the heating speed is not more than 5 ℃/min, the sintering temperature is 1150-1450 ℃, and the heat preservation time is 0.5-6h;
(5) After sintering, cooling along with the furnace to obtain Gd with excellent luminescence performance 2 O 2 S:Tb 3+ Fluorescent material samples.
FIG. 1 shows the prepared Gd 2 O 2 S:Tb 3+ The XRD pattern of the fluorescent material sample is consistent with the diffraction peak of the standard card PDF#26-1422, which shows that Gd is successfully synthesized 2 O 2 S phase, tb 3+ Successfully get into Gd 2 O 2 S matrix, sharp diffraction peak, high strength and high crystallinity.
FIG. 2 is a prepared Gd 2 O 2 S:Tb 3+ Photoluminescence excitation spectrum of fluorescent material sample, excitation spectrum of sample is wide band spectrum whose peak value is 292 nm.
FIG. 3 is a prepared Gd 2 O 2 S:Tb 3+ The photoluminescence emission spectrum of the fluorescent material sample has the highest emission peak at 544nm under 292nm ultraviolet excitation, and has bright green light emission.
FIG. 4 shows the prepared Gd 2 O 2 S:Tb 3+ The cathodoluminescence spectrum of the fluorescent material sample, shows that the sample has the highest green emission peak at 544nm under excitation by cathode rays.
FIG. 5 compares Gd with different sintering aids 2 O 2 S:Tb 3+ Photoluminescence excitation spectrum of fluorescent material sample, KCl, liF and K 3 PO 4 The three additives are added singly, doubly and doubly to enhance the excitation characteristics.
FIG. 6 compares Gd with different sintering aids 2 O 2 S:Tb 3+ Photoluminescence emission spectra of fluorescent material samples, KCl, liF and K 3 PO 4 The three auxiliary agents are added singly, doubly and doubly to enhance the emission intensity.
FIG. 7 compares Gd with different sintering aids 2 O 2 S:Tb 3+ Cathode ray emission spectra of fluorescent material samples, KCl, liF and K 3 PO 4 The three auxiliary agents are added singly, added doubly and added three times to enhance the emission characteristic, and the luminous intensity is enhanced by more than 200 percent.
Claims (1)
1. Enhancement Gd 2 O 2 S:Tb 3+ Fluorescent material excitation and luminescenceThe method for the intensity of the radio spectrum is characterized by comprising the following steps: by Gd 2 O 3 、Gd 2 (SO 4 ) 3 ·8H 2 O, C powder and Tb 4 O 7 By introducing KCl, liF and K as raw materials 3 PO 4 Three sintering aids realize enhanced luminescence, and Gd is obtained by calcining C powder at 1150-1450 ℃ for 0.5-6h in a reducing atmosphere provided by the C powder by using a double-carbon reduction technology 2 O 2 S:Tb 3+ The fluorescence material, excitation and emission spectrum intensity is enhanced.
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|---|---|---|---|---|
| US4507560A (en) * | 1980-06-13 | 1985-03-26 | Gte Products Corporation | Terbium-activated gadolinium oxysulfide X-ray phosphor |
| JPH03269085A (en) * | 1990-03-20 | 1991-11-29 | Toshiba Corp | Fluorescent material and cathode-ray tube |
| CN1111603A (en) * | 1994-01-26 | 1995-11-15 | 西门子公司 | Method for producing lightening material with high translucency |
| CN101024770A (en) * | 2007-01-30 | 2007-08-29 | 中国科学院上海硅酸盐研究所 | Method for preparing rare-earth sulfur oxide cuminous materials |
| CN101486909A (en) * | 2009-02-16 | 2009-07-22 | 昆明理工大学 | Green phosphor and preparation thereof |
| CN114162847A (en) * | 2021-12-21 | 2022-03-11 | 安徽光智科技有限公司 | Preparation method of gadolinium oxysulfide powder |
| CN115216300A (en) * | 2021-04-20 | 2022-10-21 | 中国科学院理化技术研究所 | Preparation method of trivalent terbium-doped gadolinium oxysulfide luminescent material, product and application thereof |
| CN115321579A (en) * | 2022-08-18 | 2022-11-11 | 北京科技大学 | Preparation method of high-performance sulfur oxide fluorescent powder |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1489640B1 (en) * | 2002-03-28 | 2013-07-17 | Kabushiki Kaisha Toshiba | X-ray image tube, x-ray image tube device and x-ray device |
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- 2023-04-28 CN CN202310481821.0A patent/CN116496788B/en active Active
Patent Citations (8)
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| US4507560A (en) * | 1980-06-13 | 1985-03-26 | Gte Products Corporation | Terbium-activated gadolinium oxysulfide X-ray phosphor |
| JPH03269085A (en) * | 1990-03-20 | 1991-11-29 | Toshiba Corp | Fluorescent material and cathode-ray tube |
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| Title |
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