CN101265098B - Transparent ceramic scintillator material by using lutecium oxide-gadolinium oxide solid solution as substrate and preparation method thereof - Google Patents

Transparent ceramic scintillator material by using lutecium oxide-gadolinium oxide solid solution as substrate and preparation method thereof Download PDF

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CN101265098B
CN101265098B CN200810011236XA CN200810011236A CN101265098B CN 101265098 B CN101265098 B CN 101265098B CN 200810011236X A CN200810011236X A CN 200810011236XA CN 200810011236 A CN200810011236 A CN 200810011236A CN 101265098 B CN101265098 B CN 101265098B
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transparent ceramic
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CN101265098A (en
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李晓东
孙旭东
刘妍
修稚萌
李继光
霍地
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Northeastern University China
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Abstract

一种以氧化镥和氧化钆固溶体为基质材料的透明陶瓷闪烁体材料及其制备方法，本发明包括粉体合成、成型、素烧、烧结以及退火处理等工艺步骤。本发明制备的以氧化镥-氧化钆固溶体为基质材料的透明陶瓷闪烁体材料，可见光直线透过率＞60％、机械性能良好，可用作闪烁体基质材料，本发明不但可以进一步提高氧化钆基质对电离辐射的阻断能力，提高Gd2O3的闪烁性能，还可以降低Lu2O3的生产成本，在闪烁辐射探测等领域具有应用前景。A transparent ceramic scintillator material with lutetium oxide and gadolinium oxide solid solution as matrix materials and a preparation method thereof, the invention includes the process steps of powder synthesis, molding, bisque firing, sintering and annealing treatment. The transparent ceramic scintillator material with lutetium oxide-gadolinium oxide solid solution as the matrix material prepared by the present invention has a visible light linear transmittance>60% and good mechanical properties, and can be used as a scintillator matrix material. The ability of the matrix to block ionizing radiation can improve the scintillation performance of Gd 2 O 3 , and can also reduce the production cost of Lu 2 O 3 , which has application prospects in scintillation radiation detection and other fields.

Description

It with lutecium oxide-gadolinium oxide solid solution transparent ceramic scintillator material of matrix and preparation method thereof
Technical field
The invention belongs to field of material preparation, being specifically related to a kind of is the transparent ceramic scintillator material and preparation method thereof of matrix with lutecium oxide-gadolinium oxide solid solution.
Background technology
Scintillation material is a kind ofly can absorb high energy particle or ray and send the material of optical photon, is widely used in fields such as high energy physics (as accurate electromagnetic calorimeter), nuclear medicine (as X-CT, PET and γ camera), industry (CT flaw detection), space physics, geological prospectings.Although different application can propose different requirements to scintillator, but scintillator all is used to detect ionizing rays in the overwhelming majority uses, so require scintillator high blocking ability will be arranged, promptly require scintillator to have high-density and contain the big element of ordination number to ionizing rays.In many application, therefore the large usage quantity of scintillator, also needs scintillator that cheap price is arranged, but high quality, produces in large quantity and process.
Lutecium oxide has high density (9.42g/cm 3) and high ordination number (71), this makes it quite high to the stopping power of all kinds of rays (x ray, gamma-rays); Lu 2O 3Band gap very wide (6.5eV) can hold many activator ions such as Eu as the luminescent material matrix between valence band and conduction band, Tb, and Tm, the emission level of Er etc., so lutecium oxide enjoys people to favor as the scintillator substrate material.As the Lu of the 5%Eu that mixes 2O 3The light output of base transparent flickering body is approximately 50%CsI:Tl, is applicable to the X ray digital imagery.But lutecium oxide has limited its widespread use owing to cost an arm and a leg.
Gadolinium sesquioxide has higher density (7.6g/cm equally 3) and effective atomic number (64), X ray is had very high receptivity, and cheap, have actual application value as the scintillator substrate material.But Gd 2O 3Have very high fusing point (2673K), be difficult to have practical value and get monocrystalline by the melting method preparation.In addition, because Gd 2O 3Take place to make it be difficult at high temperature be prepared into crystalline ceramics cube to the monocline phase transformation at～1200 ℃ by the pressureless sintering technology.Limited its application in the flash detection field.Up to the present, also it is not prepared into patent, the bibliographical information of crystalline ceramics by the pressureless sintering technology.In gadolinium sesquioxide matrix, be doped into a certain amount of lutecium oxide, can be expected to obtain crystalline ceramics by sintering with the gadolinium sesquioxide cube temperature increase that arrives the monocline phase transformation to more than the sintering temperature.Lutecium oxide mixed make the solid solution matrix material in the gadolinium sesquioxide, not only can further improve the blocking ability of gadolinium sesquioxide matrix, improve Gd ionizing rays 2O 3Scintillation properties, can also reduce Lu 2O 3Production cost, obtain a kind of scintillator substrate material of high comprehensive performance.
Summary of the invention
The objective of the invention is to adopt that pressureless sintering prepares a kind of highdensity transparent ceramic glaring material that has in vacuum or the hydrogen, relate in particular to lutecium oxide-gadolinium oxide solid solution transparent ceramic and preparation method thereof.
Lutecium oxide-the gadolinium oxide solid solution transparent ceramic glaring material of the present invention's preparation, its general formula is Gd 2-2x-2yLu 2xRE 2yO 3, wherein, 0.15＜x＜1,0＜y＜0.3, x, y are atomic mole fraction, RE is dopant ion Eu, Tb, one or both among Nd, Yb, the Pr.
Of the present invention is the high-density transparent ceramic scintillator material and preparation method thereof of matrix with lutecium oxide-gadolinium oxide solid solution, comprises following processing step:
1, synthetic: synthetic high sintering activity Gd 2-2x-2yLu 2xRE 2yO 3Nano-powder comprises following processing step:
(a) press composition formula Gd 2-2x-2yLu 2xRE 2yO 3Form preparation mother liquor with nitrate;
(b) adopting concentration is 0.5molL -1～2molL -1Ammonium bicarbonate aqueous solution as precipitation agent;
(c) employing prepares the precursor powder with the forward volumetry that precipitation agent splashes into mother liquor, and the pH value after the control precipitin reaction is between 5～7, and titration finishes the back and continues stirring 4h;
(d) the precursor powder obtains oxide powder after washing, drying, calcining;
The washing process parameter is: throw out is washed, to remove the foreign ion that precipitation surface is adhered to; After washing 3～4 times, throw out is soaked 24h with dehydrated alcohol or acetone,, obtain finely disseminated precursor powder to remove the Surface Physical planar water;
The drying process parameter is: will wash good precursor powder and put into drying baker, temperature is 50～120 ℃, and the time is 24h;
The calcining process parameter is: the precursor powder after will drying is put into corundum crucible after grinding in mortar, calcines 1～6 hour down for 800～1100 ℃ in temperature, makes oxide powder;
2, moulding: adopt punching block bidirectional pressed moulding or cold isostatic compaction, with oxide powder compression moulding, pressing pressure is 100～300MPa, makes biscuit;
3, biscuiting: biscuit is put into the biscuiting of van-type stove, 1200～1400 ℃ of biscuiting temperature, biscuiting is 4～24 hours under air or oxygen atmosphere;
4, sintering: the biscuit that biscuiting is good is put into the vacuum oven sintering, 1600～1800 ℃ of sintering temperatures, and sintering time 5～24 hours, vacuum tightness is not less than 1 * 10 -2MPa makes the crystalline ceramics work in-process;
5, anneal: the crystalline ceramics work in-process are put into cabinet-type electric furnace anneal, 1000～1400 ℃ of annealing temperatures, under air or oxygen atmosphere, annealing time 4～24 hours, the high-density transparent ceramic scintillator material density that makes is at 8.0-9.0g/cm 3Between, become with chemical constitution;
Can prepare lutecium oxide-gadolinium oxide solid solution transparent ceramic according to technology of the present invention, can be used as the scintillator substrate material at visible-range straight line transmitance height (＞60%), satisfactory mechanical property.
Description of drawings
Fig. 1: Gd 2-2x-2yLu 2xRE 2yO 3X ray diffracting spectrum after 1000 ℃ of calcinings of precursor powder
Fig. 2: 800 ℃ of calcining Gd 2-2x-2yLu 2xRE 2yO 3The SEM pattern photo of powder
Fig. 3: 1700 ℃ of sintering Gd 2-2x-2yLu 2xRE 2yO 3The outward appearance photo of sample
Fig. 4: 1700 ℃ of sintering Gd 2-2x-2yLu 2xRE 2yO 3Sample XRD figure spectrum
Fig. 5: Gd 2-2x-2yLu 2xRE 2yO 3The emmission spectrum of crystalline ceramics
Embodiment
Embodiment 1
1, high sintering activity Gd 2-2x-2yLu 2xRE 2yO 3Nano-powder is synthetic:
(a) with analytically pure Lu 2O 3, Gd 2O 3And Eu 2O 3Meal is dissolved in respectively in the analytical pure concentrated nitric acid solution, is mixed with 0.5molL after the filtration -1Nitrate solution, measure Gadolinium trinitrate 350ml, lutecium nitrate 125ml, europium nitrate 25ml, compound concentration is 0.5molL -1Nitrate mother liquor 500ml;
(b) preparation 0.5molL -1NH 4HCO 3Solution is as precipitation agent;
(c) 0.5molL -1NH 4HCO 3It is 0.5molL that solution splashes into 500ml concentration -1In the rare earth nitrate mother liquor, rate of addition is 3mlmin -1Between the reaction period, magnetic agitation is carried out on titration limit, limit, control terminal point pH=5, and titration finishes the back and continues to stir 4h;
(d) the precursor powder obtains oxide powder after washing, drying, calcining;
The washing process parameter is: throw out is washed, to remove the foreign ion that precipitation surface is adhered to; After washing 3～4 times, throw out is soaked 24h with dehydrated alcohol or acetone,, obtain finely disseminated precursor powder to remove the Surface Physical planar water;
The drying process parameter is: will wash good precursor powder and put into drying baker, and dry 24h down at 50 ℃;
The calcining process parameter is: the precursor powder after will drying is put into corundum crucible after grinding in mortar, at 800 ℃ of calcining 1h, makes oxide powder;
2, moulding: adopt punching block bidirectional pressed moulding or cold isostatic compaction, oxide powder is pressed into biscuit, pressing pressure is 100MPa, and the base substrate diameter after the compacting is 13mm, and thickness is 3mm;
3, biscuiting: biscuit is gone in the van-type stove to burn base substrate 1200 ℃ of pre-burnings 4 hours in resistance furnace;
4, sintering: biscuit is put into the vacuum oven sintering, and base substrate places 1600 ℃ of insulations of vacuum oven 5h, vacuum tightness 1 * 10 -2MPa makes the crystalline ceramics work in-process;
5, anneal: the crystalline ceramics work in-process are put into cabinet-type electric furnace anneal, under air or oxygen atmosphere, anneal in cabinet-type electric furnace, temperature is 1000 ℃, and 4 hours time, the high-density transparent ceramic scintillator material density that makes is 8.0g/cm 3
Embodiment 2
1, high sintering activity Gd 2-2x-2yLu 2xRE 2yO 3Nano-powder is synthetic:
(a) with analytically pure Lu 2O 3, Gd 2O 3And Tb 2O 3Meal is dissolved in respectively in the analytical pure concentrated nitric acid solution, is mixed with 0.5molL after the filtration -1Nitrate solution, Gadolinium trinitrate 300ml, lutecium nitrate 175ml, Terbium trinitrate 25ml, compound concentration are 0.5molL -1Nitrate mother liquor 500ml;
(b) preparation 1.0molL -1NH 4HCO 3Solution is as precipitation agent;
(c) 1.0molL -1NH 4HCO 3It is 0.5molL that solution splashes into 500ml concentration -1In the rare earth nitrate mother liquor, rate of addition is 3mlmin -1Between the reaction period, magnetic agitation is carried out on titration limit, limit, control terminal point pH=5.7, and titration finishes the back and continues to stir 4h;
(d) the precursor powder obtains oxide powder after washing, drying, calcining;
The washing process parameter is: throw out is washed, to remove the foreign ion that precipitation surface is adhered to; After washing 3～4 times, throw out is soaked 24h with dehydrated alcohol or acetone, removing the Surface Physical planar water,
Obtain finely disseminated precursor powder;
The drying process parameter is: will wash good precursor powder and put into drying baker, and dry 24h down at 70 ℃;
The calcining process parameter is: the precursor powder after will drying is put into corundum crucible after grinding in mortar, at 900 ℃ of calcining 2.7h, makes oxide powder;
2, moulding: adopt punching block bidirectional pressed moulding or cold isostatic compaction, oxide powder is pressed into biscuit, pressing pressure is 170MPa.Base substrate diameter after the compacting is 13mm, and thickness is 3mm;
3, biscuiting: biscuit is put into the van-type stove burn, base substrate 1270 ℃ of pre-burnings 11 hours in resistance furnace;
4, sintering: biscuit is put into the vacuum oven sintering, and base substrate places 1670 ℃ of insulations of vacuum oven 11h, vacuum tightness 2 * 10 -2MPa makes the crystalline ceramics work in-process;
5, anneal: the crystalline ceramics work in-process are put into cabinet-type electric furnace anneal, under air or oxygen atmosphere, anneal in cabinet-type electric furnace, temperature is 1130 ℃, and 11 hours time, the high-density transparent ceramic scintillator material density that makes is 8.3g/cm 3
Embodiment 3
1, high sintering activity Gd 2-2x-2yLu 2xRE 2yO 3Nano-powder is synthetic:
(a) with analytically pure Lu 2O 3, Gd 2O 3And Yb 2O 3Meal is dissolved in respectively in the analytical pure concentrated nitric acid solution, is mixed with 0.5molL after the filtration -1Nitrate solution, measure Gadolinium trinitrate 250ml, lutecium nitrate 225ml, ytterbium nitrate 25ml, compound concentration is 0.5molL -1Nitrate mother liquor 500ml;
(b) preparation 1.5molL -1NH 4HCO 3Solution is as precipitation agent;
(c) 1.5molL -1NH 4HCO 3It is 0.5molL that solution splashes into 500ml concentration -1In the rare earth nitrate mother liquor, rate of addition is 3mlmin -1Between the reaction period, magnetic agitation is carried out on titration limit, limit, control terminal point pH=6.4, and titration finishes the back and continues to stir 4h;
(d) the precursor powder obtains oxide powder after washing, drying, calcining;
The washing process parameter is: throw out is washed, to remove the foreign ion that precipitation surface is adhered to; After washing 3～4 times, throw out is soaked 24h with dehydrated alcohol or acetone,, obtain finely disseminated precursor powder to remove the Surface Physical planar water;
The drying process parameter is: will wash good precursor powder and put into drying baker, and dry 24h down at 90 ℃;
The calcining process parameter is: the precursor powder after will drying is put into corundum crucible after grinding in mortar, at 1000 ℃ of calcining 4.4h, makes oxide powder;
2, moulding: adopt punching block bidirectional pressed moulding or cold isostatic compaction, oxide powder is pressed into biscuit, pressing pressure is 200MPa.Base substrate diameter after the compacting is 13mm, and thickness is 3mm;
3, biscuiting: biscuit is put into the van-type stove burn, base substrate 1300 ℃ of pre-burnings 14 hours in resistance furnace; 4, sintering: biscuit is put into the vacuum oven sintering, and base substrate places 1700 ℃ of insulations of vacuum oven 15h, vacuum tightness 3 * 10 -2MPa makes the crystalline ceramics work in-process;
5, anneal: the crystalline ceramics work in-process are put into cabinet-type electric furnace anneal, under air or oxygen atmosphere, anneal in cabinet-type electric furnace, temperature is 1200 ℃, and 14 hours time, the high-density transparent ceramic scintillator material density that makes is 8.5g/cm 3
Embodiment 4
1, high sintering activity Gd 2-2x-2yLu 2xRE 2yO 3Nano-powder is synthetic:
(a) with analytically pure Lu 2O 3, Gd 2O 3And Nd 2O 3Meal is dissolved in respectively in the analytical pure concentrated nitric acid solution, is mixed with 0.5molL after the filtration -1Nitrate solution, measure Gadolinium trinitrate 200ml, lutecium nitrate 275ml, neodymium nitrate 25ml compound concentration is 0.5molL -1Nitrate mother liquor 500ml;
(b) preparation 1.7molL -1NH 4HCO 3Solution is as precipitation agent;
(c) 1.7molL -1NH 4HCO 3It is 0.5molL that solution splashes into 500ml concentration -1In the rare earth nitrate mother liquor, rate of addition is 3mlmin -1Between the reaction period, magnetic agitation is carried out on titration limit, limit, control terminal point pH=6.5, and titration finishes the back and continues to stir 4h;
(d) the precursor powder obtains oxide powder after washing, drying, calcining;
The washing process parameter is: throw out is washed, to remove the foreign ion that precipitation surface is adhered to; After washing 3～4 times, throw out is soaked 24h with dehydrated alcohol or acetone,, obtain finely disseminated precursor powder to remove the Surface Physical planar water;
The drying process parameter is: will wash good precursor powder and put into drying baker, and dry 24h down at 100 ℃;
The calcining process parameter is: the precursor powder after will drying is put into corundum crucible after grinding in mortar, at 1000 ℃ of calcining 5h, makes oxide powder;
2, moulding: adopt punching block bidirectional pressed moulding or cold isostatic compaction, oxide powder is pressed into biscuit, pressing pressure is 250MPa.Base substrate diameter after the compacting is 13mm, and thickness is 3mm;
3, biscuiting: biscuit is put into the van-type stove burn, base substrate 1350 ℃ of pre-burnings 19 hours in resistance furnace;
4, sintering: biscuit is put into the vacuum oven sintering, and base substrate places 1750 ℃ of insulations of vacuum oven 19h, vacuum tightness 4 * 10 -2MPa makes the crystalline ceramics work in-process;
5, anneal: the crystalline ceramics work in-process are put into cabinet-type electric furnace anneal, under air or oxygen atmosphere, anneal in cabinet-type electric furnace, temperature is 1300 ℃, and 19 hours time, the high-density transparent ceramic scintillator material density that makes is 8.7g/cm 3
Embodiment 5
1, high sintering activity Gd 2-2x-2yLu 2xRE 2yO 3Nano-powder is synthetic:
(a) with analytically pure Lu 2O 3, Gd 2O 3, Pr 2O 3And Eu 2O 3Meal is dissolved in respectively in the analytical pure concentrated nitric acid solution, is mixed with 0.5molL after the filtration -1Nitrate solution, measure Gadolinium trinitrate 200ml, lutecium nitrate 275ml, praseodymium nitrate 5ml, europium nitrate 20ml compound concentration is 0.5molL -1Nitrate mother liquor 500ml;
(b) preparation 2.0molL -1NH 4HCO 3Solution is as precipitation agent;
(c) 2.0molL -1NH 4HCO 3It is 0.5molL that solution splashes into 500ml concentration -1In the rare earth nitrate mother liquor, rate of addition is 3mlmin -1Between the reaction period, magnetic agitation is carried out on titration limit, limit, control terminal point pH=7, and titration finishes the back and continues to stir 4h;
(d) the precursor powder obtains oxide powder after washing, drying, calcining;
The washing process parameter is: throw out is washed, to remove the foreign ion that precipitation surface is adhered to; After washing 3～4 times, throw out is soaked 24h with dehydrated alcohol or acetone,, obtain finely disseminated precursor powder to remove the Surface Physical planar water;
The drying process parameter is: will wash good precursor powder and put into drying baker, and dry 24h down at 120 ℃;
The calcining process parameter is: the precursor powder after will drying is put into corundum crucible after grinding in mortar, at 1100 ℃ of calcining 6h, makes oxide powder;
2, moulding: adopt punching block bidirectional pressed moulding or cold isostatic compaction, oxide powder is pressed into biscuit, pressing pressure is 300MPa.Base substrate diameter after the compacting is 13mm, and thickness is 3mm;
3, biscuiting: biscuit is put into the van-type stove burn, base substrate 1400 ℃ of pre-burnings 24 hours in resistance furnace;
4, sintering: biscuit is put into the vacuum oven sintering, and base substrate places 1800 ℃ of insulations of vacuum oven 24h, vacuum tightness 4 * 10 -2MPa makes the crystalline ceramics work in-process;
5, anneal: the crystalline ceramics work in-process are put into cabinet-type electric furnace anneal, under air or oxygen atmosphere, anneal in cabinet-type electric furnace, temperature is 1400 ℃, and 24 hours time, the high-density transparent ceramic scintillator material density that makes is 9.0g/cm 3

Claims (4)

1.一种以氧化镥-氧化钆固溶体为基质的透明陶瓷闪烁体材料，其特征在于化学组成为Gd2-2x-2yLu2xRE2yO3，其中，0.15＜x＜1，0＜y＜0.3，x、y为原子摩尔分数，式中RE为掺杂离子Eu、Tb、Nd、Yb、Pr中的一种或两种。1. A transparent ceramic scintillator material based on lutetium oxide-gadolinium oxide solid solution, characterized in that the chemical composition is Gd 2-2x-2y Lu 2x RE 2y O 3 , wherein, 0.15<x<1, 0<y <0.3, x, y are atomic mole fractions, where RE is one or two of dopant ions Eu, Tb, Nd, Yb, Pr. 2.按权利要求1所述的以氧化镥-氧化钆固溶体为基质的透明陶瓷闪烁体材料，其密度在8.0-9.0g/cm3之间，随化学组成变化而变。2. The transparent ceramic scintillator material based on lutetium oxide-gadolinium oxide solid solution according to claim 1, the density of which is between 8.0-9.0 g/cm 3 , which varies with the chemical composition. 3.按权利要求1所述的氧化镥-氧化钆固溶透明陶瓷闪烁体材料的制备方法，其特征在于包括以下步骤：3. by the preparation method of lutetium oxide-gadolinium oxide solid solution transparent ceramic scintillator material according to claim 1, it is characterized in that comprising the following steps: (1)制备高烧结活性的Gd2-2x-2yLu2xRE2yO3纳米粉体；(1) Preparation of Gd 2-2x-2y Lu 2x RE 2y O 3 nanopowder with high sintering activity; (2)采用钢模双向压制成型或冷等静压成型，压制压力为100～300MPa，将纳米粉体成型，获得素坯；(2) Two-way compression molding or cold isostatic pressing with a steel mold, the compression pressure is 100-300MPa, and the nano-powder is molded to obtain a biscuit; (3)素坯在空气或氧气气氛下素烧4～24小时，素烧温度1200～1400℃；(3) The biscuit is bisque-fired under air or oxygen atmosphere for 4-24 hours, and the bisque-fired temperature is 1200-1400°C; (4)素烧后，将素坯真空烧结5～24小时，真空度大于或等于1×10-2MPa，获得透明陶瓷样品；(4) After bisque firing, vacuum sinter the green body for 5 to 24 hours, and the vacuum degree is greater than or equal to 1×10 -2 MPa to obtain a transparent ceramic sample; (5)烧结的陶瓷样品在空气中或氧气气氛中退火，退火温度为1000～1400℃，时间4～24小时。(5) The sintered ceramic sample is annealed in air or in an oxygen atmosphere at an annealing temperature of 1000-1400° C. for 4-24 hours. 4.按权利3要求所述的氧化镥-氧化钆固溶透明陶瓷闪烁体材料的制备方法，其特征在于所述的高烧结活性Gd2-2x-2yLu2xRE2yO3纳米粉体采取如下步骤制备：4. According to the preparation method of the lutetium oxide-gadolinium oxide solid-solution transparent ceramic scintillator material described in claim 3, it is characterized in that the described high sintering activity Gd 2-2x-2y Lu 2x RE 2y O 3 nanometer powder adopts Prepare as follows: (1)按组成式Gd2-2x-2yLu2xRE2yO3以硝酸盐的形式配制母液；(1) Prepare the mother liquor in the form of nitrate according to the composition formula Gd 2-2x-2y Lu 2x RE 2y O 3 ; (2)采用浓度为0.5M～2M的碳酸氢铵水溶液作为沉淀剂；(2) Adopting a concentration of ammonium bicarbonate aqueous solution of 0.5M to 2M as a precipitating agent; (3)采用将沉淀剂滴入母液的正向滴定法制备先驱物粉体，控制沉淀反应后的pH值在5～7之间；(3) The precursor powder is prepared by dropping the precipitant into the mother liquor by forward titration, and the pH value after the precipitation reaction is controlled between 5 and 7; (4)先驱物粉体经洗涤、干燥、煅烧后获得氧化物粉体。煅烧温度在800～1100℃，时间在1～6小时。(4) The oxide powder is obtained after the precursor powder is washed, dried and calcined. The calcination temperature is 800-1100° C., and the time is 1-6 hours.
CN200810011236XA 2008-04-30 2008-04-30 Transparent ceramic scintillator material by using lutecium oxide-gadolinium oxide solid solution as substrate and preparation method thereof Expired - Fee Related CN101265098B (en)

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