CN101955773A - Praseodymium and cerium-doped lutetium scandium borate luminous material and preparation method thereof - Google Patents

Praseodymium and cerium-doped lutetium scandium borate luminous material and preparation method thereof Download PDF

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CN101955773A
CN101955773A CN201010501533XA CN201010501533A CN101955773A CN 101955773 A CN101955773 A CN 101955773A CN 201010501533X A CN201010501533X A CN 201010501533XA CN 201010501533 A CN201010501533 A CN 201010501533A CN 101955773 A CN101955773 A CN 101955773A
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cerium
doped lutetium
lutetium scandium
praseodymium
crystal
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任国浩
吴云涛
丁栋舟
潘尚可
杨帆
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention relates to the field of scintillating crystals or fluorescent powder materials, and provides a praseodymium and cerium-doped lutetium scandium borate scintillating crystal or praseodymium and cerium-doped lutetium scandium borate fluorescent powder and a preparation method. The material has the chemical formula of (Lu1-mScm)1-x-yCexPryBO3, wherein x is more than or equal to 0.0001 and less than or equal to 0.05; y is more than or equal to 0.0001 and less than or equal to 0.01; and m is more than or equal to 0.1 and less than or equal to 0.5. After Pr<3+> ions are added into a luminous material cerium-doped lutetium scandium borate, the praseodymium and cerium-doped lutetium scandium borate scintillating single crystal and the fluorescent powder of the invention are synthesized by a Czochrolski method and a high-temperature solid state method respectively; and compared with the cerium-doped lutetium scandium borate scintillating crystal or the fluorescent powder not doped with the Pr<3+> ions, the cerium-doped lutetium scandium borate doped with the Pr<3+> ions has the luminous efficiency which is improved by 40 to 50 percent so as to remarkably improve the luminous efficiency of the cerium-doped lutetium scandium borate material.

Description

The borate doped lutetium scandium of a kind of praseodymium cerium luminescent material and preparation method thereof
Technical field
The present invention relates to scintillation crystal or fluorescent powder material field, be specifically related to a kind of praseodymium cerium borate doped lutetium scandium scintillation crystal or fluorescent material and preparation method thereof.
Background technology
(chemical formula is LuBO to the boric acid lutetium 3) crystal is a kind of scintillation crystal of finding recently, it has, and physical and chemical performance is good, and transparency range is wide, thereby it is particularly suitable for doing the matrix of Ce ion doping excellent performance scintillation crystal.The scientist M.J.Weber[M.J.Weber of U.S. LBNL, S.E.Derenzo, C.DuJardin, et al.Dense Ce 3+-activated scintillatormaterials, Proceedings of Scint ' 95, pp.325-328, (Edited by P.Dorenbos and C.W.E.vanEijk) Delft, The Netherlands, 1996] pass through a series of high-density Ce 3+Point out LuBO after the research of adulterated powder material scintillation properties 3: Ce is a kind of promising novel high-performance scintillation material.U.S. scientist William Moses[W.W.Moses afterwards, et al.Recent results in a search for inorganic scintillators for X-and gamma ray detection, in:Proceedings of Scint ' 97,1997, p.358], Lyons, France first L.Zhang[L.Zhang of university, C.Pedrini, C.Madej, et al.Fast fluorescence and scintillation properties of cerium and praseodymium dopedlutetium orthoborates.Radiation Effects and Defects in Solids, 150, (1999) 47-52] etc. the people all further confirmed the scintillation properties that it is superior by the powder experiment.But up to the present never have LuBO 3: the relevant report of Ce single crystal performance, and have only LuBO 3: the report of Ce powder body material performance.As shown in the table, LuBO 3: the performance of Ce powder is compared still to have obviously with other scintillation crystal and is had superiority, and in the powder owing to have a large amount of crystal boundaries, macroscopic view or microdefect, thereby generally speaking its performance can be poorer than the single crystal material with component.Practice in the past and theoretical study results all make us have reason to infer, if can be with LuBO 3: Ce is prepared into high-quality monocrystalline, and other classical scintillation crystals of its comprehensive scintillation properties are compared can be more superior, thereby researching value is also more arranged.
Yet because LuBO 3Material itself exists serious phase transformation problem, and causes melting method to prepare very difficulty of this crystalline material.And people such as Shun-Ichi Hatamoto in 2009 are by doping Sc 3+Ion, adopting crystal pulling method successfully to prepare one-component is Lu 0.9Sc 0.1BO 3: the solid solution crystals of Ce.[Shun-Ichi Hatamoto, Takafumi Yamazaki, JunHasegawa, Masamichi Katsurayama, Motomi Oshika, Yutaka Anzai, Growth and scintillationproperties of cerium doped lutetium scandium borate single crystals, Journal of Crystal Growth311 (2009) 530-533], but simultaneously because the not enough BGO crystalline 60% of its photoyield of problems such as its crystal mass.And our seminar has prepared the boric acid lutetium scandium solid solution crystals that photoyield is a BGO crystalline 130%, but its luminous efficiency still has the raising space.The praseodymium ion emission peak of having reported the borate doped lutetium of calcite phase praseodymium in the document just has overlapping [L.Guerbous with the cerium ion excitation peak of the borate doped lutetium material of cerium; O.Krachni.Luminescence of Ce 3+Traces in Pr 3+-doped LuBO 3And YBO 3Orthoborates.Radiation Effects and Defects in Solids 161 (2010) 199-206].Same we find at Lu 1-mSc mBO 3In the matrix, Pr 3+The emission wavelength scope just and Ce 3+Excitation wavelength range have overlapping.Under energetic ray such as X ray or gamma-ray exciting, Pr 3+And Lu 1-mSc mBO 3Matrix is simultaneously to Ce 3+Produce excitation, can improve Lu 1-mSc mBO 3: the luminous efficiency of Ce.
Summary of the invention
The object of the present invention is to provide the borate doped lutetium scandium of a kind of praseodymium cerium luminescent material, by the Pr that in the borate doped lutetium scandium of cerium material, mixes 3+, to improve its luminous efficiency effectively.
The present invention adopts following technical scheme to solve above-mentioned technical problem:
The borate doped lutetium scandium of a kind of praseodymium cerium luminescent material is characterized in that the chemical formula of this material is (Lu 1-mSc m) 1-x-yCe xPr yBO 3, wherein: 0.0001≤x≤0.05,0.0001≤y≤0.01,0.1≤m≤0.5.
Above-mentioned chemical formula (Lu 1-mSc m) 1-x-yCe xPr yBO 3In, the relation of the molar ratio between the corresponding chemical element in the molecule all represented in bottom right mark numeral and letter.
Preferably, 0.005≤x≤0.02,0.001≤y≤0.01,0.1≤m≤0.3.
Preferable, the borate doped lutetium scandium of described praseodymium cerium luminescent material is praseodymium cerium borate doped lutetium scandium scintillation single crystal or fluorescent material.
The present invention also provides the preparation method of described praseodymium cerium borate doped lutetium scandium scintillation single crystal or fluorescent material, and wherein: the borate doped lutetium scandium of praseodymium cerium scintillation single crystal can be prepared with crystal pulling method; The borate doped lutetium scandium of praseodymium cerium fluorescent material can prepare with high temperature solid-state method.
Adopt crystal pulling method to prepare the borate doped lutetium scandium of praseodymium cerium scintillation single crystal, may further comprise the steps:
(1) batching: press chemical formula (Lu 1-mSc m) 1-x-yCe xPr yBO 3In stoichiometric ratio, with Lu 2O 3, H 3BO 3, contain the Ce compound and contain the Pr compound after, carry out pre-burning, to remove H wherein 2O and CO 2
(2) sintering: the raw material after the pre-burning in the step 1) is pressed into the material ingot, carries out presintering in 800～1300 ℃ then, make the polycrystal ingot;
(3) crystal growth: will expect that ingot and seed crystal put into lifting furnace and carry out crystal growth, the control pull rate is 0.1-5mm/h, and speed of rotation is 3-20rpm;
(4) cooling: after crystal growth finishes, in 10～200 hours, drop to room temperature, obtain the borate doped lutetium scandium of praseodymium cerium scintillation single crystal.
Preferable, in the step 1), as long as be controlled at can be with water in the raw material and co 2 removal, as raw material being carried out pre-burning under 100～300 ℃ air atmosphere for the temperature of pre-burning.Preferably, the described Ce of containing compound is CeO 2, containing the Pr compound is Pr 6O 11
Preferable, step 2) in: the concrete steps that raw material are pressed into the material ingot are: in the sealed vessel of packing into behind the compound thorough mixing, depress to fine and close material ingot with the pressure that waits static pressure at 90～300Mpa; The described agglomerating time is 5～200 hours.
Preferable, in the described step 3), crystal growth is carried out under protective atmosphere.Preferably, described protective atmosphere is neutral atmosphere or weak oxide atmosphere, as high pure nitrogen, argon gas or air.
Preferably, described seed crystal is boric acid lutetium scandium, the borate doped lutetium scandium of cerium, the borate doped lutetium scandium of praseodymium or praseodymium cerium boric acid lutetium scandium.
Preferably, described lifting furnace is the Medium frequency induction lifting furnace.
Adopt high temperature solid-state method to prepare the borate doped lutetium scandium of cerium fluorescent material, may further comprise the steps:
(1) batching: press chemical formula (Lu 1-mSc m) 1-x-yCe xPr yBO 3In stoichiometric ratio, with Lu 2O 3, H 3BO 3, contain the Ce compound and contain the Pr compound after, carry out pre-burning to remove H wherein 2O and CO 2
(2) sintering: the raw material after the pre-burning in the step 1) is pressed into the material ingot, carries out presintering in 800～1300 ℃ then;
(3) grind: after sintering is finished, take out sample and grind, obtain the borate doped lutetium scandium of praseodymium cerium fluorescent material.
Preferable, in the step 1), as long as be controlled at can be with water in the raw material and co 2 removal, as raw material being carried out pre-burning under 100～300 ℃ air atmosphere for the temperature of pre-burning.Preferably, the described Ce of containing compound is CeO 2, containing the Pr compound is Pr 6O 11
Preferable, described step 2) in, the agglomerating time is 5～200 hours.
The present invention is the extra Pr that adds in the borate doped lutetium scandium of luminescent material cerium 3+Ion has synthesized praseodymium cerium borate doped lutetium scandium scintillation single crystal and fluorescent material respectively by crystal pulling method and high temperature solid-state method, and does not mix Pr 3+Cerium borate doped lutetium scandium scintillation crystal or fluorescent material compare doping Pr 3+After the luminous efficiency of the borate doped lutetium scandium of cerium can improve 40～50%, obviously improved the luminous efficiency of the borate doped lutetium scandium of cerium material.
Description of drawings
Fig. 1 is the burst of ultraviolel spectrum (room temperature) of embodiment 1 prepared luminescent material; (310nm, 340nm) and also have praseodymium ion excitation peak (230nm), this explanation praseodymium cerium ion exists transmission ofenergy can to find corresponding to the luminous excitation wavelength of cerium ion typical cerium ion excitation peak is arranged not only from collection of illustrative plates.
Fig. 2 is embodiment 1 prepared (Lu 0.8Sc 0.2) 0.985Ce 0.01Pr 0.005BO 3(the Lu of the luminescent material and the praseodymium that do not mix 0.8Sc 0.2) 0.99Ce 0.01BO 3The excitation of X-rays emission spectrum of luminescent material is (room temperature) relatively.By (Lu behind the doping praseodymium ion 0.8Sc 0.2) 0.99Ce 0.01BO 3Luminous efficiency improves about 50%.
Embodiment
Embodiment 1
(Lu 0.8Sc 0.2) 0.989Ce 0.01Pr 0.001BO 3The preparation of fluorescent material:
(1) raw material is Lu 2O 3, H 3BO 3, CeO 2And Pr 6O 11, purity is 4N.Under the air atmosphere at 200 ℃ of pre-burning raw materials, the H that removes 2O and CO 2, be Lu in molar ratio 2O 3: Sc 2O 3: H 3BO 3: Ce 2O 3: Pr 2O 3=0.3956: 0.0989: 1: 0.005: 0.0005 prepares burden, CeO 2With Pr 6O 11Weight by waiting Ce and the principle that waits the Pr molar weight to convert.
(2) in the mould with the Φ 20mm that packs into behind the raw material thorough mixing, moulding on hand-operated hydraulic press, pressure is 20MPa, takes out the material ingot, puts into the high temperature retort furnace and synthesizes.Synthesis temperature is 1000 ℃, and sintering time is 20 hours.
(3) after sintering is finished, take out sample, grind then, just made (Lu 0.8Sc 0.2) 0.989Ce 0.01Pr 0.001BO 3BO 3Fluorescent material.
Present embodiment gained scintillation single crystal gets the excitation of X-rays emission spectrum as shown in Figure 2 through X ray test.The excitation of X-rays spectrum is carried out integration by wavelength, and its integrated intensity can be used for characterizing the strong and weak relatively of its luminous efficiency.As shown in Figure 2, by integration (Lu as can be seen 0.8Sc 0.2) 0.985Ce 0.01Pr 0.005BO 3The luminous efficiency of sample is than (the Lu under the same test condition 0.8Sc 0.2) 0.989Ce 0.01BO 3The luminous efficiency of sample improves about 50%.
Embodiment 2
(Lu 0.8Sc 0.2) 0.985Ce 0.01Pr 0.005BO 3The preparation of fluorescent material:
(1) raw material is Lu 2O 3, H 3BO 3, CeO 2And Pr 6O 11, purity is 4N.Under the air atmosphere at 200 ℃ of pre-burning raw materials, the H that removes 2O and CO 2, be Lu in molar ratio 2O 3: Sc 2O 3: H 3BO 3: Ce 2O 3: Pr 2O 3=0.394: 0.0985: 1: 0.005: 0.0025 prepares burden, CeO 2With Pr 6O 11Weight by waiting Ce and the principle that waits the Pr molar weight to convert.
(2) in the mould with the Φ 20mm that packs into behind the raw material thorough mixing, moulding on hand-operated hydraulic press, pressure is 20MPa, takes out the material ingot, puts into the high temperature retort furnace and synthesizes.Synthesis temperature is 1000 ℃, and sintering time is 20 hours.
(3) after sintering is finished, take out sample, grind then, just made (Lu 0.8Sc 0.2) 0.985Ce 0.01Pr 0.005BO 3Fluorescent material.
Detect through X ray, with the excitation of X-rays emission spectrum relatively, present embodiment gained (Lu 0.8Sc 0.2) 0.985Ce 0.01Pr 0.005BO 3The fluorescent material sample than (Lu 0.8Sc 0.2) 0.99Ce 0.01BO 3The luminous efficiency of fluorescent material sample improve about 40%.
Embodiment 3
(Lu 0.8Sc 0.2) 0.989Ce 0 01Pr 0.001BO 3The Czochralski grown of scintillation single crystal:
(1) raw material is Lu 2O 3, H 3BO 3, CeO 2And Pr 6O 11, purity is 4N.Under the air atmosphere at 200 ℃ of pre-burning raw materials, the H that removes 2O and CO 2, be Lu in molar ratio 2O 3: Sc 2O 3: H 3BO 3: Ce 2O 3: Pr 2O 3=0.3956: 0.0989: 1: 0.005: 0.0005 prepares burden, CeO 2With Pr 6O 11Weight by waiting Ce and the principle that waits the Pr molar weight to convert.
(2) seal in the plastics tubing with the Φ 30mm that packs into behind the raw material thorough mixing, depress to fine and close material ingot, in retort furnace, carry out presintering with the pressure that waits static pressure at 200Mpa.1100 ℃ of sintering temperatures, sintering time is 10 hours, makes the polycrystal ingot.
(3) fall the material ingot and be transferred to Φ 50 * 30mm 3The Ir pot in, growth atmosphere is an Ar gas.Be equipped with suitable insulation construction, inoculation, the seed crystal preheating, the seed crystal that will rotate is then introduced melt, and is little molten.On the basis of setting up the thermograde that is complementary with pull rate, beginning lifts (being respectively 10rpm and 2mm/h) with certain rotating speed speed, and by last weighing control system adjustment melt temperature, through necking down, shouldering, isometrical and ending waits the stage, obtains the crystal of desired size, at last crystal is pulled away from liquid level.
(4) cooling dropped to room temperature totally in 20 hours.(the Lu that obtains 0.8Sc 0.2) 0.989Ce 0.01Pr 0.001BO 3Monocrystalline, equal-diameter part are Φ 15 * 30mm 3
To present embodiment gained scintillation single crystal (Lu 0.8Sc 0.2) 0.989Ce 0.01Pr 0.001BO 3(Lu with the same sample size 0.8Sc 0.2) 0.99Ce 0.01BO 3Sample carries out X ray and detects, through the excitation of X-rays emission spectrum relatively, and (Lu 0.8Sc 0.2) 0.989Ce 0.01Pr 0.001BO 3Single crystal samples than (Lu 0.8Sc 0.2) 0.99Ce 0.01BO 3The luminous efficiency increase rate of single crystal samples suitable with corresponding fluorescent samples.
Embodiment 4
(Lu 0.8Sc 0.2) 0.985Ce 0.01Pr 0.005BO 3The Czochralski grown of scintillation single crystal:
(1) raw material is Lu 2O 3, H 3BO 3, CeO 2And Pr 6O 11, purity is 4N.Under the air atmosphere at 200 ℃ of pre-burning raw materials, the H that removes 2O and CO 2, be Lu in molar ratio 2O 3: Sc 2O 3: H 3BO 3: Ce 2O 3: Pr 2O 3=0.394: 0.0985: 1: 0.005: 0.0025 prepares burden, CeO 2With Pr 6O 11Weight by waiting Ce and the principle that waits the Pr molar weight to convert.
(2) seal in the plastics tubing with the Φ 30mm that packs into behind the raw material thorough mixing, depress to fine and close material ingot, in retort furnace, carry out presintering with the pressure that waits static pressure at 200Mpa.1000 ℃ of sintering temperatures, sintering time is 20 hours, makes the polycrystal ingot.
(3) fall the material ingot and be transferred to Φ 50 * 30mm 3The Ir pot in, growth atmosphere is an Ar gas.Be equipped with suitable insulation construction, inoculation, the seed crystal preheating, the seed crystal that will rotate is then introduced melt, and is little molten.On the basis of setting up the thermograde that is complementary with pull rate, beginning lifts (being respectively 5rpm and 0.5mm/h) with certain rotating speed speed, and by last weighing control system adjustment melt temperature, through necking down, shouldering, isometrical and ending waits the stage, obtains the crystal of desired size, at last crystal is pulled away from liquid level.
(5) cooling dropped to room temperature totally in 20 hours.(the Lu that obtains 0.8Sc 0.2) 0.985Ce 0.01Pr 0.005BO 3Monocrystalline, equal-diameter part are Φ 15 * 30mm 3
To present embodiment gained scintillation single crystal (Lu 0.8Sc 0.2) 0.985Ce 0.01Pr 0.005BO 3(Lu with the same sample size 0.8Sc 0.2) 0.99Ce 0.01BO 3Sample carries out X ray and detects, through the excitation of X-rays emission spectrum relatively, and ((Lu 0.8Sc 0.2) 0.985Ce 0.01Pr 0.005BO 3Single crystal samples than (Lu 0.8Sc 0.2) 0.99Ce 0.01BO 3The luminous efficiency increase rate and the fluorescent samples of single crystal samples suitable.

Claims (8)

1. the borate doped lutetium scandium of a praseodymium cerium luminescent material is characterized in that the chemical formula of this material is (Lu 1-mSc m) 1-x-yCe xPr yB0 3, wherein: 0.0001≤x≤0.05,0.0001≤y≤0.01,0.1≤m≤0.5.
2. the borate doped lutetium scandium of praseodymium cerium as claimed in claim 1 luminescent material is characterized in that 0.005≤x≤0.02,0.001≤y≤0.01,0.1≤m≤0.3.
3. the borate doped lutetium scandium of praseodymium cerium as claimed in claim 1 or 2 luminescent material is characterized in that, the borate doped lutetium scandium of described praseodymium cerium luminescent material is scintillation single crystal or fluorescent material.
4. as the preparation method of the borate doped lutetium scandium of the described praseodymium cerium of arbitrary claim among claim 1-3 luminescent material, it is characterized in that the borate doped lutetium scandium of praseodymium cerium scintillation single crystal is prepared with crystal pulling method; The borate doped lutetium scandium of praseodymium cerium fluorescent material prepares with high temperature solid-state method.
5. preparation method as claimed in claim 4 is characterized in that, adopts crystal pulling method to prepare the borate doped lutetium scandium of praseodymium cerium scintillation single crystal, may further comprise the steps:
1) batching: press chemical formula (Lu 1-mSc m) 1-x-yCe xPr yBO 3In stoichiometric ratio, with Lu 2O 3, H 3BO 3, contain the Ce compound with contain the Pr compound after, carry out pre-burning;
2) sintering: the raw material after the pre-burning in the step 1) is pressed into the material ingot, carries out presintering in 900～1300 ℃ then, make the polycrystal ingot;
3) crystal growth: will expect that ingot and seed crystal put into lifting furnace and carry out crystal growth, the control pull rate is 0.1-5mm/h, and speed of rotation is 3-20rpm;
4) cooling: after crystal growth finishes, in 10～200 hours, drop to room temperature, obtain the borate doped lutetium scandium of praseodymium cerium scintillation single crystal.
6. preparation method as claimed in claim 4 is characterized in that, adopts high temperature solid-state method to prepare the borate doped lutetium scandium of cerium fluorescent material, may further comprise the steps:
1) batching: press chemical formula (Lu 1-mSc m) 1-x-yCe xPr yBO 3In stoichiometric ratio, with Lu 2O 3, H 3BO 3, contain the Ce compound with contain the Pr compound after, carry out pre-burning;
2) sintering: the raw material after the pre-burning in the step 1) is pressed into the material ingot, carries out presintering in 800～1300 ℃ then;
3) grind: after sintering is finished, take out sample and grind, obtain the borate doped lutetium scandium of praseodymium cerium fluorescent material.
7. as claim 5 or 6 described preparation methods, it is characterized in that the described Ce of containing compound is CeO 2, containing the Pr compound is Pr 6O 11
8. as claim 5 or 6 described preparation methods, it is characterized in that described step 2) in, the time of presintering is 5～200 hours.
CN201010501533XA 2010-10-09 2010-10-09 Praseodymium and cerium-doped lutetium scandium borate luminous material and preparation method thereof Pending CN101955773A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101949061A (en) * 2010-10-29 2011-01-19 中国科学院上海硅酸盐研究所 Rare earth-doped lutetium-scandium borate scintillation single crystals and growth method thereof
CN112180083A (en) * 2020-09-30 2021-01-05 厦门稀土材料研究所 IgM antibody detection kit, detection card thereof and preparation method of detection card
CN115367766A (en) * 2022-08-05 2022-11-22 广东省科学院资源利用与稀土开发研究所 Lithium sodium lutetium borate, rare earth doped compound and crystal thereof, and preparation method and application thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101949061A (en) * 2010-10-29 2011-01-19 中国科学院上海硅酸盐研究所 Rare earth-doped lutetium-scandium borate scintillation single crystals and growth method thereof
CN101949061B (en) * 2010-10-29 2012-05-30 中国科学院上海硅酸盐研究所 Rare earth-doped lutetium-scandium borate scintillation single crystals and growth method thereof
CN112180083A (en) * 2020-09-30 2021-01-05 厦门稀土材料研究所 IgM antibody detection kit, detection card thereof and preparation method of detection card
CN115367766A (en) * 2022-08-05 2022-11-22 广东省科学院资源利用与稀土开发研究所 Lithium sodium lutetium borate, rare earth doped compound and crystal thereof, and preparation method and application thereof
CN115367766B (en) * 2022-08-05 2023-06-13 广东省科学院资源利用与稀土开发研究所 Lithium sodium lutetium borate, rare earth doped compound and crystal thereof, and preparation method and application thereof
WO2024027106A1 (en) * 2022-08-05 2024-02-08 广东省科学院资源利用与稀土开发研究所 Lithium sodium lutetium borate, rare earth doped compound and crystal thereof, preparation method therefor, and use thereof

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Application publication date: 20110126