CN101270283A - Gadolinium lutetium oxide fluorescent powder and preparation method thereof - Google Patents

Gadolinium lutetium oxide fluorescent powder and preparation method thereof Download PDF

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CN101270283A
CN101270283A CNA2008100614489A CN200810061448A CN101270283A CN 101270283 A CN101270283 A CN 101270283A CN A2008100614489 A CNA2008100614489 A CN A2008100614489A CN 200810061448 A CN200810061448 A CN 200810061448A CN 101270283 A CN101270283 A CN 101270283A
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lutetium oxide
fluorescent powder
gadolinium lutetium
oxide fluorescent
preparation
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秦来顺
舒康颖
史宏声
田光磊
吴云涛
柴文祥
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China Jiliang University
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China Jiliang University
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Abstract

The invention discloses gadolinium oxide and lutecia phosphor powder and a preparation method thereof. The phosphor powder is solid solution of Eu<3+> mixed with Gd2O3 and Lu2O3, and is in cubic crystal structure. The solid phase sintering method is used for preparing the phosphor powder. High-purity powdered Lu2O3, Gd2O3 and Eu2O3 are accurately weighed, and are mixed uniformly, and calcined in a muffle in ordinary atmosphere; finally, the mixture is cooled, thus getting the cubic gadolinium oxide and lutecia phosphor powder mixed with Eu<3+>. The phosphor powder emits red light when being activated by ultraviolet light or X ray, and can be used as the phosphor powder of CRT, PDP, LED and FED, and an X-ray scintillating material.

Description

Gadolinium lutetium oxide fluorescent powder and preparation method thereof
Technical field
The present invention relates to functional materials and technology of preparing thereof, be specifically related to a kind of light-emitting phosphor material and preparation method thereof.
Background technology
Rare earth ion Eu 3+Adulterated cube of phase Gd 2O 3It is a kind of very important luminous and scintillation material.Just study its characteristics of luminescence as far back as Bril in 1964 and Wanmaker, be subjected to people's extensive concern in recent years as fluorescent material and thin-film material.As red fluorescence powder efficiently, has important application prospects in fields such as plasma imaging, high definition television, projection TV, flat pannel display.As scintillator, Gd 2O 3: Eu is a kind of ceramic scintillator of high comprehensive performance, in high resolution X-CT, X ray safety check imaging device and CCD coupling large area x-ray imaging field very important application prospect will be arranged.Gd 2O 3Has high-density (7.64g/cm 3), high effective atomic number (Zeff=64), so it is very strong to X ray and gamma-ray receptivity, between Lu 2O 3And LuAG (Lu 3Al 5O 12) between, far above Y 2O 3: Eu and (Y, Gd) 2O 3: Eu also is higher than Gd 2O 2S:Pr; Gd 2O 3: the luminous efficiency of Eu is very high, and its twinkling light is output as 18465 ± 5000ph./MeV during the film attitude, with Lu 2O 3: Eu is suitable; Gd 2O 3: the luminous predominant wavelength of Eu is 610nm, and is good with the photorectifier coupling, detection efficiency height, and UFC (Gd 2O 2S:Pr) predominant wavelength is positioned at 510nm, and the efficient of photorectifier has only 40%～50%, the optical detection weak effect; Gd during 10ms under excitation of X-rays 2O 3: the twilight sunset of Eu is 10-3 (0.1%), by adding Tb 3+Plasma can reduce time of persistence.In addition, Gd 2O 3Chemical property is stable, satisfactory mechanical property.
Because Gd 2O 3: the Eu cost of material is cheap, the luminescent properties brilliance, and market outlook are good, however because Gd 2O 3There is structural phase transition at 1250 ℃, Gd under the low temperature 2O 3Belong to body-centered cubic structure (C type), be higher than 1250 ℃ and change monocline (Type B) into, and have only the Gd of cube phase 2O 3: Eu just has high luminous efficiency, so will obtain the Gd of cube phase 2O 3: Eu fluorescent material needs lower temperature, and lower synthesis temperature makes its degree of crystallinity poor, and luminous intensity is low.For overcoming Gd 2O 3Phase transformation, the synthetic big phosphor material powder of luminous intensity has only Gd under higher temperature 2O 3Be prepared into the presoma calcining or add suitable doping agent and suppress phase transformation.Precursor process has increased synthesis technique, has increased bigger cost, and common employed chemical process can increase environmental pollution.
Lu 2O 3: Eu is another very potential red light flourescent material, excellent property, yet Lu 2O 3Prices of raw and semifnished materials costliness, price are high always, use so hindered its market.And Lu 2O 3With a cube Gd 2O 3Have identical crystalline structure, and the similarity on the formed compound property of rare earth element, so study the phosphor material powder that the two formed sosoloid is expected to obtain more superior, the cheap high comprehensive performance of luminescent properties.
Summary of the invention
The present invention is taking all factors into consideration Lu 2O 3: Eu and cube Gd 2O 3: on the basis of Eu performance and price, the speciality of two kinds of materials of performance forms a kind of new gadolinium lutetium oxide sosoloid fluorescent material, the object of the present invention is to provide a kind of phosphor material powder and preparation method thereof.
The technical scheme that the present invention solves its technical problem employing is:
1) gadolinium lutetium oxide fluorescent powder:
This fluorescent material is Eu 3+Adulterated Gd 2O 3With Lu 2O 3Sosoloid, chemical constitution is Gd 2 (1-x-y)Lu 2xEu 2yO 3, 0.3≤x≤0.9,0.01≤y≤0.15 wherein; The crystalline structure of this material is the vacant fluorite structure of isometric system, and spacer is Ia3.
Described Gd 2 (1-x-y)Lu 2xEu 2yO 3In add the Nd of 0.001wt%～1wt% again 3+, Tb 3+, Pr 3+
2) preparation method of gadolinium lutetium oxide fluorescent powder:
Prepare the method that fluorescent material adopts solid state sintering, adopt Lu 2O 3, Gd 2O 3And Eu 2O 3Powder is a starting raw material, is Gd by chemical constitution 2 (1-x-y)Lu 2xEu 2yO 3, wherein after 0.3≤x≤0.9,0.01≤y≤0.15 weighing, uniform mixing is calcined in the retort furnace of common atmosphere then, drops to the normal temperature cooling at last, obtains the Eu with cube phase 3+Adulterated gadolinium lutetium oxide fluorescent powder.
Weighing is raw material batch mixing 10～24 hours in ball mill accurately.
The incinerating temperature is at 1300 ℃～1700 ℃ in retort furnace, and optimum calcinating temperature is 1600 ℃.
Gadolinium lutetium oxide fluorescent powder of the present invention and preparation method thereof has following characteristics:
1, the gadolinium lutetium oxide fluorescent powder material is a sosoloid, can make things convenient within the specific limits to regulate its chemical constitution, thereby be convenient to regulate the relevant luminescent properties of fluorescent material, as luminous intensity, fall time, twilight sunset etc.
2, at Gd 2O 3With Lu 2O 3Market value between greatest differences, under the prerequisite of satisfy using, can improve Gd during preparation fluorescent material as far as possible 2O 3Ratio, thereby reduce the cost of material.
3, gadolinium lutetium oxide fluorescent powder material all components is a rare earth oxide, and the synthesis technique that is adopted is a solid phase synthesis, and material and technology are all environmentally friendly, have development potentiality.
4, the emission wavelength of gadolinium lutetium oxide fluorescent powder is positioned at 611nm, the light that totally takes on a red color, and luminous intensity is higher than Lu 2O 3: Eu and Gd 2O 3: Eu, luminescent properties is good
5 and Gd 2O 3: Eu compares, and gadolinium lutetium oxide fluorescent powder has higher density, to the absorption and the detectivity height of x ray, has advantage in x X-ray detection X material is used.
Therefore, the gadolinium lutetium oxide fluorescent powder material that the present invention obtained sends ruddiness under ultraviolet excitation or x rays excite, can be used for CRT, PDP, LED, FED fluorescent material, is particularly suitable for as x ray scintillation detecting material.
Description of drawings
Fig. 1 is with Lu 2O 3And Gd 2O 3X x ray diffration pattern x for raw material solid state reaction product.
Fig. 2 contains different Eu 3+The burst of ultraviolel luminescent spectrum of gadolinium lutetium oxide fluorescent powder.
Fig. 3 is that Lu/Re is to mixing 5at%Eu 3+The influence of luminous intensity of gadolinium lutetium oxide.
Fig. 4 is Eu 3+Doping is the influence of luminous intensity of the gadolinium lutetium oxide of 30at% to Lu content.
Embodiment
Gadolinium lutetium oxide fluorescent powder is Eu 3+Adulterated Gd 2O 3With Lu 2O 3Sosoloid, its chemical constitution can be expressed as Gd 2 (1-x-y)Lu 2xEu 2yO 3, wherein highly purified Lu is adopted in 0.3≤x≤0.98,0.01≤y≤0.15 during the synthetizing phosphor powder material 2O 3, Gd 2O 3, Eu 2O 3Powder is a starting raw material, carries out proportioning according to this stoichiometric ratio, for the luminescent properties (comprising persistence characteristic, luminous intensity and fall time etc.) that improves material, adds the Nd of 0.001wt%～1wt% when preparing burden 3+, Tb 3+, Pr 3+, suppress the generation of twilight sunset with these rare earth ions, or accelerate decay of luminescence, if increase such ion certainly, the luminous intensity of gadolinium lutetium oxide fluorescent powder will reduce.
Behind accurate feed proportioning, mixing raw material to be packed in the ball mill, batch mixing 10～24 hours increases mixing time raw material is mixed, and makes raw material carry out solid state reaction and is more prone to, and can react fully between each component.
Prepare the method that fluorescent material adopts solid state sintering.With the mixed raw materials alumina crucible of packing into, perhaps in platinum, in the retort furnace of common atmosphere, calcine, calcining temperature is at 1300 ℃～1700 ℃, optimum calcinating temperature is 1600 ℃, and soaking time is 2～20 hours, and best soaking time is 5 hours, concrete soaking time and initial feed have confidential relation, depend mainly on the granularity and the specific surface area of initial feed.After the raw material cooling cooling after the calcining, the Eu that can obtain to have cube phase 3+Adulterated gadolinium lutetium oxide fluorescent powder, but temperature-fall period temperature programmed control cooling, but also naturally cooling.
The synthetic gadolinium lutetium oxide fluorescent powder is carried out the x ray diffraction, and the result shows that the crystalline structure of material is the vacant fluorite structure of isometric system, and spacer is Ia3, is not new crystalline structure, is Gd 2O 3With Lu 2O 3The sosoloid that forms is with Gd 2O 3Low temperature cube phase and Lu 2O 3Structure identical, difference only is the difference of lattice parameter.The result of x ray material phase analysis shows simultaneously, works as Lu 2O 3Content when being lower than 30at%, synthetic product is cube phase and monocline mixture mutually, non-gadolinium lutetium oxide sosoloid of the present invention, and work as Lu 2O 3Content when surpassing 30at%, synthetic product is a gadolinium lutetium oxide sosoloid, the result as shown in Figure 1.
Eu 3+The burst of ultraviolel emmission spectrum of adulterated gadolinium lutetium oxide as shown in Figure 2, under the 263nm ultraviolet excitation, the luminous predominant wavelength of gadolinium lutetium oxide is positioned at the ruddiness bands of a spectrum of 611nm, and the luminous intensity of gadolinium lutetium oxide clocklike changes with Lu content therein, and Lu/Re is to mixing 5at%Eu 3+The influence of luminous intensity of gadolinium lutetium oxide see that shown in the accompanying drawing 3, Re is a rare earth total in the sosoloid, comprise Gd, Lu and Eu, as seen along with the increase of Lu/Re ratio, i.e. the raising of Lu content, the total trend of total luminous intensity is reducing.
Eu 3+Be the luminous active ions of gadolinium lutetium oxide, the influence luminous to material is very big, and accompanying drawing 4 is Eu 3+Doping is the influence of luminous intensity of the gadolinium lutetium oxide of 30at% to Lu content, as can be seen from the figure, and along with Eu 3+Increase, luminous intensity increases earlier, reduces then, weight break point is near～7%.
Embodiment 1:
The preparation gadolinium lutetium oxide fluorescent powder, its chemical constitution can be expressed as Gd 1.3Lu 0.6Eu 0.1O 3, adopt highly purified Lu during the synthetizing phosphor powder material 2O 3, Gd 2O 3, Eu 2O 3Powder is a starting raw material, and raw material sources are adsorptive type rare earth ore deposit in the Ganzhou, and purity is 99.99%, carries out proportioning according to this stoichiometric ratio.Behind accurate feed proportioning, mixing raw material is packed in the ball mill into batch mixing 24 hours.Adopt the method for solid state sintering, with the mixed raw materials alumina crucible of packing into, calcine in the retort furnace of common atmosphere, calcining temperature is 1300 ℃, and soaking time is 10 hours.After the raw material cooling cooling after the calcining, the Eu that can obtain to have cube phase 3+Adulterated gadolinium lutetium oxide fluorescent powder, naturally cooling.The synthetic gadolinium lutetium oxide fluorescent powder is carried out the x ray diffraction, the result shows that the crystalline structure of material is the vacant fluorite structure of isometric system, spacer is Ia3, its burst of ultraviolel emmission spectrum as shown in Figure 2, under the 263nm ultraviolet excitation, the luminous predominant wavelength of gadolinium lutetium oxide is positioned at the ruddiness bands of a spectrum of 611nm.
Embodiment 2:
The preparation gadolinium lutetium oxide fluorescent powder, its chemical constitution can be expressed as Gd 0.98Lu 1.0Eu 0.02O 3, adopt highly purified Lu during the synthetizing phosphor powder material 2O 3, Gd 2O 3, Eu 2O 3Powder is a starting raw material, and raw material sources are adsorptive type rare earth ore deposit in the Ganzhou, and purity is 99.99%, carries out proportioning according to this stoichiometric ratio.Behind accurate feed proportioning, mixing raw material is packed in the ball mill into batch mixing 10 hours.Adopt the method for solid state sintering, with the mixed raw materials alumina crucible of packing into, calcine in the retort furnace of common atmosphere, calcining temperature is 1600 ℃, and soaking time is 10 hours.After the raw material cooling cooling after the calcining, the Eu that can obtain to have cube phase 3+Adulterated gadolinium lutetium oxide fluorescent powder, naturally cooling.The synthetic gadolinium lutetium oxide fluorescent powder is carried out the x ray diffraction, the result shows that the crystalline structure of material is the vacant fluorite structure of isometric system, spacer is Ia3, its burst of ultraviolel emmission spectrum as shown in Figure 2, under the 263nm ultraviolet excitation, the luminous predominant wavelength of gadolinium lutetium oxide is positioned at the ruddiness bands of a spectrum of 611nm.
Embodiment 3:
The preparation gadolinium lutetium oxide fluorescent powder, its chemical constitution can be expressed as Gd 1.1Lu 0.6Eu 0.3O 3, adopt highly purified Lu during the synthetizing phosphor powder material 2O 3, Gd 2O 3, Eu 2O 3Powder is a starting raw material, and raw material sources are adsorptive type rare earth ore deposit in the Ganzhou, and purity is 99.99%, carries out proportioning according to this stoichiometric ratio.Behind accurate feed proportioning, mixing raw material is packed in the ball mill into batch mixing 20 hours.Adopt the method for solid state sintering, with the mixed raw materials alumina crucible of packing into, calcine in the retort furnace of common atmosphere, calcining temperature is 1700 ℃, and soaking time is 10 hours.After the raw material cooling cooling after the calcining, the Eu that can obtain to have cube phase 3+Adulterated gadolinium lutetium oxide fluorescent powder, naturally cooling.The synthetic gadolinium lutetium oxide fluorescent powder is carried out the x ray diffraction, and the result shows that the crystalline structure of material is the vacant fluorite structure of isometric system, and spacer is Ia3, its luminous intensity and the different Eu that mix 3+The gadolinium lutetium oxide material of concentration more as shown in Figure 4.
Embodiment 4:
The preparation gadolinium lutetium oxide fluorescent powder, its chemical constitution can be expressed as Gd 0.1Lu 1.8Eu 0.1O 3, adopt highly purified Lu during the synthetizing phosphor powder material 2O 3, Gd 2O3, Eu 2O 3Powder is a starting raw material, carries out proportioning according to this stoichiometric ratio, and raw material sources are adsorptive type rare earth ore deposit in the Ganzhou, and purity is 99.99%, in order to improve the luminescent properties of material, adds the Pr of 0.001wt% when preparing burden 3+Suppress the generation of twilight sunset.Behind accurate feed proportioning, mixing raw material is packed in the ball mill into batch mixing 24 hours.Adopt the method for solid state sintering, with the mixed raw materials platinum crucible of packing into, calcine in the retort furnace of common atmosphere, calcining temperature is at 1500 ℃, and soaking time is 5 hours, after the raw material cooling cooling after the calcining, and the Eu that can obtain to have cube phase 3+Adulterated gadolinium lutetium oxide fluorescent powder.
The synthetic gadolinium lutetium oxide fluorescent powder is carried out the x ray diffraction, and the result shows that the crystalline structure of material is the vacant fluorite structure of isometric system, and spacer is Ia3, is Gd 2O 3With Lu 2O 3The sosoloid that forms, Gd 0.1Lu 1.8Eu 0.1O 3The burst of ultraviolel emmission spectrum as shown in Figure 2, under the 263nm ultraviolet excitation, the luminous predominant wavelength of gadolinium lutetium oxide is positioned at the ruddiness bands of a spectrum of 611nm.

Claims (5)

1, a kind of gadolinium lutetium oxide fluorescent powder is characterized in that: this fluorescent material is Eu 3+Adulterated Gd 2O 3With Lu 2O 3Sosoloid, chemical constitution is Gd 2 (1-x-y)Lu 2xEu 2yO 3, 0.3≤x≤0.9,0.01≤y≤0.15 wherein; The crystalline structure of this material is the vacant fluorite structure of isometric system, and spacer is Ia3.
2, a kind of gadolinium lutetium oxide fluorescent powder according to claim 1 is characterized in that: described Gd 2 (1-x-y)Lu 2xEu 2yO 3In add the Nd of 0.001wt%～1wt% again 3+, Tb 3+, Pr 3+
3, be used for the preparation method of the described a kind of gadolinium lutetium oxide fluorescent powder of claim 1, it is characterized in that: prepare the method that fluorescent material adopts solid state sintering, adopt Lu 2O 3, Gd 2O 3And Eu 2O 3Powder is a starting raw material, is Gd by chemical constitution 2 (1-x-y)Lu 2xEu 2yO 3, wherein after 0.3≤x≤0.9,0.01≤y≤0.15 weighing, uniform mixing is calcined in the retort furnace of common atmosphere then, drops to the normal temperature cooling at last, obtains the Eu with cube phase 3+Adulterated gadolinium lutetium oxide fluorescent powder.
4, the preparation method of a kind of gadolinium lutetium oxide fluorescent powder according to claim 3 is characterized in that: weighing is raw material batch mixing 10～24 hours in ball mill accurately.
5, the preparation method of a kind of gadolinium lutetium oxide fluorescent powder according to claim 3 is characterized in that: the incinerating temperature is at 1300 ℃～1700 ℃ in retort furnace, and optimum calcinating temperature is 1600 ℃.
CNA2008100614489A 2008-04-30 2008-04-30 Gadolinium lutetium oxide fluorescent powder and preparation method thereof Pending CN101270283A (en)

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Cited By (10)

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WO2010078224A2 (en) * 2008-12-30 2010-07-08 Saint-Gobain Ceramics & Plastics, Inc. Ceramic scintillator body and scintillation device
CN102234508A (en) * 2010-04-20 2011-11-09 中国科学院上海硅酸盐研究所 Rare-earth-doped lutetium borate radiation detection material, and preparation and application thereof
US8872119B2 (en) 2008-12-30 2014-10-28 Saint-Gobain Ceramics & Plastics, Inc. Ceramic scintillator body and scintillation device
US8877093B2 (en) 2008-12-30 2014-11-04 Saint-Gobain Ceramics & Plastics, Inc. Ceramic scintillator body and scintillation device
US9183962B2 (en) 2008-12-30 2015-11-10 Saint-Gobain Ceramics & Plastics, Inc. Ceramic scintillator body and scintillation device
CN105238400A (en) * 2015-11-20 2016-01-13 济南大学 Novel mono-dispersed spherical rare earth oxide fluorescent powder ad preparation method thereof
CN110156021A (en) * 2019-05-31 2019-08-23 承德石油高等专科学校 A kind of SiNWS:Eu3+,Lu3+Fluorescent nano material preparation method
CN114507521A (en) * 2022-02-25 2022-05-17 中国计量大学 Broadband scintillator and X-ray imaging application thereof
CN115215651A (en) * 2022-01-09 2022-10-21 上海御光新材料科技股份有限公司 Preparation method of rare earth doped lutetium oxide based composite luminescent ceramic
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Cited By (15)

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US8877093B2 (en) 2008-12-30 2014-11-04 Saint-Gobain Ceramics & Plastics, Inc. Ceramic scintillator body and scintillation device
US9183962B2 (en) 2008-12-30 2015-11-10 Saint-Gobain Ceramics & Plastics, Inc. Ceramic scintillator body and scintillation device
CN102317409B (en) * 2008-12-30 2016-01-20 圣戈本陶瓷及塑料股份有限公司 Ceramic scintillator body and flashing device
CN102317409A (en) * 2008-12-30 2012-01-11 圣戈本陶瓷及塑料股份有限公司 Ceramic scintillator body and scintillation device
US20120085972A1 (en) * 2008-12-30 2012-04-12 Centre National De La Recherche Scientifique Ceramic scintillator body and scintillation device
US8872119B2 (en) 2008-12-30 2014-10-28 Saint-Gobain Ceramics & Plastics, Inc. Ceramic scintillator body and scintillation device
WO2010078224A3 (en) * 2008-12-30 2010-09-16 Saint-Gobain Ceramics & Plastics, Inc. Ceramic scintillator body and scintillation device
US9175216B2 (en) 2008-12-30 2015-11-03 Saint-Gobain Ceramics & Plastics, Inc. Ceramic scintillator body and scintillation device
WO2010078224A2 (en) * 2008-12-30 2010-07-08 Saint-Gobain Ceramics & Plastics, Inc. Ceramic scintillator body and scintillation device
CN102234508A (en) * 2010-04-20 2011-11-09 中国科学院上海硅酸盐研究所 Rare-earth-doped lutetium borate radiation detection material, and preparation and application thereof
CN105238400A (en) * 2015-11-20 2016-01-13 济南大学 Novel mono-dispersed spherical rare earth oxide fluorescent powder ad preparation method thereof
CN110156021A (en) * 2019-05-31 2019-08-23 承德石油高等专科学校 A kind of SiNWS:Eu3+,Lu3+Fluorescent nano material preparation method
CN115215651A (en) * 2022-01-09 2022-10-21 上海御光新材料科技股份有限公司 Preparation method of rare earth doped lutetium oxide based composite luminescent ceramic
CN114507521A (en) * 2022-02-25 2022-05-17 中国计量大学 Broadband scintillator and X-ray imaging application thereof
CN115490517A (en) * 2022-10-17 2022-12-20 闽都创新实验室 Red light flashing ceramic and preparation method and application thereof

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