CN101818057A - Luminous material and preparation method thereof - Google Patents
Luminous material and preparation method thereof Download PDFInfo
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- CN101818057A CN101818057A CN201010171891A CN201010171891A CN101818057A CN 101818057 A CN101818057 A CN 101818057A CN 201010171891 A CN201010171891 A CN 201010171891A CN 201010171891 A CN201010171891 A CN 201010171891A CN 101818057 A CN101818057 A CN 101818057A
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Abstract
本发明提供了一种发光材料，具有以通式(I)表示的原子比组成：LiSr4(BO3)3∶Cex(I)；其中，0.007≤x≤0.008。本发明还提供了一种发光材料的制备方法，包括：将硼酸或氧化硼与碳酸锂、碳酸锶和氧化铈混合，在空气气氛中预烧，其中氧化铈与碳酸锶的摩尔比x满足条件：0.007≤x≤0.008；将预烧后的混合物在还原气氛中烧结，得到发光材料。与现有技术相比，本发明提供了的材料吸收辐射能之后的热释发光曲线仅由一个温度为482K时的发光峰组成，峰温适当，有利于热释光信号的存储；该发光峰峰型较好，且发光强度较高，有利于辐射剂量信号的测试。
The present invention provides a luminescent material having an atomic ratio composition represented by the general formula (I): LiSr 4 (BO 3 ) 3 : Cex (I); wherein, 0.007≤x≤0.008. The present invention also provides a method for preparing a luminescent material, comprising: mixing boric acid or boron oxide with lithium carbonate, strontium carbonate and cerium oxide, and pre-firing in an air atmosphere, wherein the molar ratio x of cerium oxide to strontium carbonate satisfies the condition : 0.007≤x≤0.008; sintering the pre-fired mixture in a reducing atmosphere to obtain a luminescent material. Compared with the prior art, the thermoluminescence curve of the material provided by the present invention after absorbing radiation energy only consists of a luminescence peak at a temperature of 482K, and the peak temperature is appropriate, which is conducive to the storage of thermoluminescence signals; the luminescence peak The peak shape is better and the luminous intensity is higher, which is conducive to the test of radiation dose signals.
Description
Technical field
The present invention relates to the luminescent material technical field, relate in particular to a kind of light emitting borate material and preparation method thereof.
Background technology
The thermoluminescence of material is meant the thermoluminescence of material after absorbed radiation energy, can predict radiation dose in certain zone according to its luminous quantity.At present, the thermoluminescence dosimeter by the thermoluminescence material preparation has been widely used in numerous areas such as radio-protective, radiation therapy, environmental monitoring, measurement in geological age, archaeology, space flight.
Prior art discloses the multiple thermoluminescence material that is used for thermoluminescence dosimeter, as LiF, CaSO
4, CaF
2, LiB
4O
7Deng.Wherein, LiF is owing to having erosion resistance, abrasion resistance, being insoluble in water and fading rate is low at normal temperatures etc. that characteristics become the most frequently used thermoluminescent dosemeter material.Cameron and colleague thereof develop a kind of main LiF material TLD100 (LiF:Mg by magnesium and titanium activator, Ti), thermoluminescence twinkler as standard obtains widespread use (A.G.Kozakiewicz, A.T.Davidson, D.J.Wilkinsin, The effect of pre-irradiation annealing on TL glow curves of LiF (Mg), Nucl.Instrum.Meth.Phys.Res.B, 2000,166,577-580).But, LiF:Mg, the thermoluminescence sensitivity of Ti material is lower.
Prior art also discloses the LiF material of other ion dopings, as LiF:Mg, and Cu, P; LiF:Mg, Cu, Na, (K.Tang, Dependentce of thermoluminescence in LiF:Mg, Cu such as Si, Na, Si phosphor on Na dopant concentration and thermal treatment, Radiat.Meas., 2003,37,133-144.A.J.J.Bos, K.Meijvogel, J.Th.M.de Haas, P.Bilski, P.Olko, Thermoluninescence properties of LiF (Mg, Cu, P) with different copperconcentrations, Radiat.Protec.Dosim., 1996,65,199-202).These LiF materials have higher thermoluminescence sensitivity when the maximum heating temperature is no more than 270 ℃, but there are a plurality of glow peaks in the thermoluminescence peak-to-peak shape complexity of these LiF materials, is unfavorable for the test of dose signal.Simultaneously, the residual signal of this type of LiF material after high temperature is luminous is higher, has reduced precision of test result.
Summary of the invention
In view of this, technical problem to be solved by this invention is to provide a kind of luminescent material and preparation method thereof, and luminescent material provided by the invention accepts that thermoluminescence peak-to-peak shape after the radiating capacity is simple, the peak temperature suitable, helps the test of radiation dose signals.
The invention provides a kind of luminescent material, have with the atomic ratio of general formula (I) expression and form:
LiSr
4(BO
3)
3:Ce
x
(I)；
Wherein, 0.007≤x≤0.008.
The present invention also provides a kind of preparation method of luminescent material, and described luminescent material has with the atomic ratio of general formula (I) expression to be formed:
LiSr
4(BO
3)
3:Ce
x
(I)；
Described preparation method comprises:
Boric acid or boron oxide are mixed with Quilonum Retard, Strontium carbonate powder and cerium oxide, pre-burning in air atmosphere, wherein the mol ratio x of cerium oxide and Strontium carbonate powder satisfies condition: 0.007≤x≤0.008;
With the sintering in reducing atmosphere of the mixture after the pre-burning, obtain luminescent material.
Preferably, the temperature of described pre-burning is 300 ℃～550 ℃.
Preferably, the time of described pre-burning is 2h～5h.
Preferably, described agglomerating temperature is 600 ℃～1000 ℃.
Preferably, the described agglomerating time is 8h～20h.
Preferably, described reducing atmosphere is CO, H
2Or H
2And N
2Gas mixture.
Preferably, before carrying out sintering, the mixture after the pre-burning is ground.
Compared with prior art, the invention provides a kind of LiSr of having
4(BO
3)
3: Ce
xThe material that atomic ratio is formed, wherein, Ce is an activator.Glow peak when the thermoluminescence curve after the described absorbed radiating capacity only is 482K by a temperature is formed, and the peak temperature is suitable, helps the storage of thermoluminescence signal; This luminous peak-to-peak type is better, and luminous intensity is higher, helps the test of radiation dose signals.Simultaneously, described material is better to the dose response of ray, presents better linearity, has higher sensitivity.In addition, LiSr
4(BO
3)
3: Ce
xThe preparation technology of material is simple, and raw material cheaply is easy to get, low production cost.
Description of drawings
The LiSr that Fig. 1 provides for the embodiment of the invention
4(BO
3)
3: Ce
0.008The thermoluminescence luminosity curve figure of material after by gamma-ray irradiation;
The LiSr that Fig. 2 provides for the embodiment of the invention
4(BO
3)
3: Ce
0.008Material is to gamma-ray dose response curve.
Embodiment
The invention provides a kind of luminescent material, have with the atomic ratio of general formula (I) expression and form:
LiSr
4(BO
3)
3:Ce
x
(I)
Wherein, 0.007≤x≤0.008.
In general formula (I), LiSr
4(BO
3)
3Be matrix, Ce is the activator that is entrained in the matrix.
With Ce
3+Be entrained in LiSr as activator
4(BO
3)
3In the LiSr that obtains
4(BO
3)
3: Ce
xAfter the absorbing radiation, in heat-processed, gradually the energy that the absorbs form with light is discharged, determines radiation dose according to luminous intensity, thus carry out in the environment or human body in the detection of radiation dose.
Luminescent material provided by the invention the thermoluminescence, also can be used for Organic Light Emitting Diode in can be used in thermoluminescence dosimeter, independent or luminous under the exciting of UV-light or near-ultraviolet light jointly with other luminescent materials.
The present invention also provides a kind of preparation method of luminescent material, and described luminescent material has with the atomic ratio of general formula (I) expression to be formed:
LiSr
4(BO
3)
3:Ce
x
(I)；
Described preparation method comprises:
Boric acid or boron oxide are mixed with Quilonum Retard, Strontium carbonate powder and cerium oxide, pre-burning in air atmosphere, the mol ratio x of its mesoboric acid or boron oxide and Strontium carbonate powder satisfies condition: 0.007≤x≤0.008;
With the sintering in reducing atmosphere of the mixture after the pre-burning, obtain luminescent material.
Among the present invention, at first with boric acid or boron oxide with carry out pre-burning after Quilonum Retard, Strontium carbonate powder and cerium oxide mix, wherein, the mol ratio x of cerium oxide and Strontium carbonate powder satisfies condition: 0.007≤x≤0.008.Described mixing is preferably ground and mixed.
In order to obtain purer material, described lime carbonate is preferably analytical pure lime carbonate, and described Quilonum Retard is preferably the analytical pure Quilonum Retard, and described boric acid or boron oxide are preferably analytical pure boric acid or boron oxide, and it is more than 99.99% that described cerium oxide is preferably purity.
The effect of pre-burning is to remove impurities in raw materials, makes Ce
3+At LiSr
4(BO
3)
3In distribution more even so that obtain better glow peak.Among the present invention, the temperature when carrying out pre-burning in air is preferably 300 ℃-550 ℃, and the time is preferably 2h～5h.
With the sintering in reducing gas atmosphere of the mixture after the pre-burning, each raw material is reacted, generate LiSr
4(BO
3)
3: Ce
xDescribed sintering temperature is preferably 600 ℃-1000 ℃, and the time is preferably 8h～20h; Reducing atmosphere is preferably CO, H
2Or H
2And N
2Gas mixture.
For abundant sintering, the present invention preferably carried out regrinding with the mixture after the pre-burning before carrying out sintering.
Compared with prior art, the invention provides a kind of LiSr of having
4(BO
3)
3: Ce
xThe material that atomic ratio is formed, wherein, Ce is an activator.Glow peak when the thermoluminescence curve after the described absorbed radiating capacity only is 482K by a temperature is formed, and the peak temperature is suitable, helps the storage of thermoluminescence signal; This luminous peak-to-peak type is better, and luminous intensity is higher, helps the test of radiation dose signals.Simultaneously, described material is better to the dose response of ray, presents better linearity, has higher sensitivity.In addition, LiSr
4(BO
3)
3: Ce
xThe preparation technology of material is simple, and raw material cheaply is easy to get, low production cost.
In order further to understand the present invention, luminescent material provided by the invention and preparation method thereof is described in detail below in conjunction with embodiment.
Embodiment 1
Getting the analytically pure Quilonum Retard of 1mol, the analytically pure Strontium carbonate powder of 8mol, the analytically pure boric acid of 6mol and 0.064mol purity and be 99.9% cerium oxide fully grinds evenly and after the oven dry in mortar and puts into corundum crucible, in air atmosphere, pre-burning 3h under 400 ℃ temperature, obtain mixing material, after mixing material is cooled to room temperature, in mortar, fully grind once more and mix, put into corundum crucible, fill around under the condition of carbon-point, 710 ℃ roasting temperatures 16 hours, naturally cool to room temperature, obtain LiSr after in mortar, grinding
4(BO
3)
3: Ce
0.008
With LiSr
4(BO
3)
3: Ce
0.008Through 100Gy's
60The Co gamma-ray irradiation is then with 2Ks
-1Heating rate heating, obtain thermoluminescence luminosity curve figure, referring to Fig. 1, the LiSr that Fig. 1 provides for the embodiment of the invention
4(BO
3)
3: Ce
0.008The thermoluminescence luminosity curve figure of material after by gamma-ray irradiation.As shown in Figure 1, LiSr
4(BO
3)
3: Ce
0.008Glow peak when the thermoluminescence luminosity curve of material only is 482K by 1 temperature is formed.
With LiSr
4(BO
3)
3: Ce
0.008Material is respectively through 1mGy, 5mGy, 10mGy, 50mGy, 100mGy, 200mGy, 425mGy, 600mGy and 1000mGy
60The Co gamma-ray irradiation is then respectively with 20Ks
-1Heating rate heating, obtain corresponding thermoluminescence intensity, obtain the graphic representation that dosage and relatively hot are released light intensity, i.e. dose response curve figure, referring to Fig. 2, the LiSr that Fig. 2 provides for the embodiment of the invention
4(BO
3)
3: Ce
0.008Material is to gamma-ray dose response curve.As shown in Figure 2, LiSr provided by the invention
4(BO
3)
3: Ce
0.008Material presents better linearity, and linearly dependent coefficient can reach 0.999.
Embodiment 2
Getting the analytically pure Quilonum Retard of 1mol, the analytically pure Strontium carbonate powder of 8mol, the analytically pure boric acid of 6mol and 0.056mol purity and be 99.9% cerium oxide fully grinds evenly and after the oven dry in mortar and puts into corundum crucible, in air atmosphere, pre-burning 3h under 450 ℃ temperature, obtain mixing material, after mixing material is cooled to room temperature, in mortar, fully grind once more and mix, put into corundum crucible, fill around under the condition of carbon-point, 720 ℃ roasting temperatures 15 hours, naturally cool to room temperature, obtain LiSr after in mortar, grinding
4(BO
3)
3: Ce
0007
With LiSr
4(BO
3)
3: Ce
0.007Through 100Gy's
60The Co gamma-ray irradiation is then with 2Ks
-1Heating rate heating, among the thermoluminescence luminosity curve figure that obtains, the glow peak when only having 1 temperature to be 482K.
Embodiment 3
Getting the analytically pure Quilonum Retard of 1mol, the analytically pure Strontium carbonate powder of 8mol, the analytically pure boric acid of 6mol and 0.0576mol purity and be 99.9% cerium oxide fully grinds evenly and after the oven dry in mortar and puts into corundum crucible, in air atmosphere, pre-burning 2.5h under 500 ℃ temperature, obtain mixing material, after mixing material is cooled to room temperature, in mortar, fully grind once more and mix, put into corundum crucible, fill around under the condition of carbon-point, 750 ℃ roasting temperatures 12 hours, naturally cool to room temperature, obtain LiSr after in mortar, grinding
4(BO
3)
3: Ce
0.0072
With LiSr
4(BO
3)
3: Ce
0.0072Through 100Gy's
60The Co gamma-ray irradiation is then with 2Ks
-1Heating rate heating, among the thermoluminescence luminosity curve figure that obtains, the glow peak when only having 1 temperature to be 482K.
Embodiment 4
Getting the analytically pure Quilonum Retard of 1mol, the analytically pure Strontium carbonate powder of 8mol, the analytically pure boric acid of 6mol and 0.0592mol purity and be 99.9% cerium oxide fully grinds evenly and after the oven dry in mortar and puts into corundum crucible, in air atmosphere, pre-burning 3h under 400 ℃ temperature, obtain mixing material, after mixing material is cooled to room temperature, in mortar, fully grind once more and mix, put into corundum crucible, fill around under the condition of carbon-point, 710 ℃ roasting temperatures 16 hours, naturally cool to room temperature, obtain LiSr after in mortar, grinding
4(BO
3)
3: Ce
0.0074
With LiSr
4(BO
3)
3: Ce
0.0074Through 100Gy's
60The Co gamma-ray irradiation is then with 2Ks
-1Heating rate heating, among the thermoluminescence luminosity curve figure that obtains, the glow peak when only having 1 temperature to be 482K.
Embodiment 5
Getting the analytically pure Quilonum Retard of 1mol, the analytically pure Strontium carbonate powder of 8mol, the analytically pure boric acid of 6mol and 0.0608mol purity and be 99.9% cerium oxide fully grinds evenly and after the oven dry in mortar and puts into corundum crucible, in air atmosphere, pre-burning 4h under 350 ℃ temperature, obtain mixing material, after mixing material is cooled to room temperature, in mortar, fully grind once more and mix, put into corundum crucible, fill around under the condition of carbon-point, 760 ℃ roasting temperatures 18 hours, naturally cool to room temperature, obtain LiSr after in mortar, grinding
4(BO
3)
3: Ce
0.0076
With LiSr
4(BO
3)
3: Ce
0.0076Through 100Gy's
60The Co gamma-ray irradiation is then with 2Ks
-1Heating rate heating, among the thermoluminescence luminosity curve figure that obtains, the glow peak when only having 1 temperature to be 482K.
Embodiment 6
Getting the analytically pure Quilonum Retard of 1mol, the analytically pure Strontium carbonate powder of 8mol, the analytically pure boric acid of 6mol and 0.0624mol purity and be 99.9% cerium oxide fully grinds evenly and after the oven dry in mortar and puts into corundum crucible, in air atmosphere, pre-burning 4h under 350 ℃ temperature, obtain mixing material, after mixing material is cooled to room temperature, in mortar, fully grind once more and mix, put into corundum crucible, fill around under the condition of carbon-point, 760 ℃ roasting temperatures 18 hours, naturally cool to room temperature, obtain LiSr after in mortar, grinding
4(BO
3)
3: Ce
0.0078
With LiSr
4(BO
3)
3: Ce
0.0078Through 100Gy's
60The Co gamma-ray irradiation is then with 2Ks
-1Heating rate heating, among the thermoluminescence luminosity curve figure that obtains, the glow peak when only having 1 temperature to be 482K.
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (8)
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102879795A (en) * | 2012-10-11 | 2013-01-16 | 中国科学院长春应用化学研究所 | Application of KSr4(BO3)3:Ce3+ in Preparation of Electron Paramagnetic Resonance Dosimeter |
| CN102879796A (en) * | 2012-10-11 | 2013-01-16 | 中国科学院长春应用化学研究所 | Application of LiSr4(BO3)3:Ce3+ in Preparation of Electron Paramagnetic Resonance Dosimeter |
| CN103074056A (en) * | 2012-12-27 | 2013-05-01 | 陕西师范大学 | Preparation method of SrB6O10·5H2O:Eu3+ luminescent material |
| CN106590638A (en) * | 2016-11-30 | 2017-04-26 | 重庆理工大学 | Praseodymium ion-doped potassium strontium borate fluorescent powder and high-temperature solid-phase preparation method |
| CN107286933A (en) * | 2017-05-27 | 2017-10-24 | 陕西科技大学 | A kind of boric acid lanthanum-strontium base blue light fluorescent powder of cerium dopping three and preparation method thereof |
| CN108624319A (en) * | 2018-05-31 | 2018-10-09 | 杭州电子科技大学 | A kind of white light LEDs borate orange fluorescent powder and preparation method thereof |
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| CN101525535A (en) * | 2008-03-07 | 2009-09-09 | 财团法人工业技术研究院 | Borate fluorescent material and white light emitting device |
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| US20060231851A1 (en) * | 2005-04-19 | 2006-10-19 | Gelcore, Llc | Red phosphor for LED based lighting |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102879795A (en) * | 2012-10-11 | 2013-01-16 | 中国科学院长春应用化学研究所 | Application of KSr4(BO3)3:Ce3+ in Preparation of Electron Paramagnetic Resonance Dosimeter |
| CN102879796A (en) * | 2012-10-11 | 2013-01-16 | 中国科学院长春应用化学研究所 | Application of LiSr4(BO3)3:Ce3+ in Preparation of Electron Paramagnetic Resonance Dosimeter |
| CN102879795B (en) * | 2012-10-11 | 2015-02-18 | 中国科学院长春应用化学研究所 | Application of KSr4(BO3)3:Ce3+ in Preparation of Electron Paramagnetic Resonance Dosimeter |
| CN103074056A (en) * | 2012-12-27 | 2013-05-01 | 陕西师范大学 | Preparation method of SrB6O10·5H2O:Eu3+ luminescent material |
| CN103074056B (en) * | 2012-12-27 | 2015-01-28 | 陕西师范大学 | Preparation method of SrB6O10·5H2O:Eu3+ luminescent material |
| CN106590638A (en) * | 2016-11-30 | 2017-04-26 | 重庆理工大学 | Praseodymium ion-doped potassium strontium borate fluorescent powder and high-temperature solid-phase preparation method |
| CN106590638B (en) * | 2016-11-30 | 2019-03-19 | 重庆理工大学 | A kind of potassium strontium borate fluorescent powder and high-temperature solid phase preparation method adulterating praseodymium ion |
| CN107286933A (en) * | 2017-05-27 | 2017-10-24 | 陕西科技大学 | A kind of boric acid lanthanum-strontium base blue light fluorescent powder of cerium dopping three and preparation method thereof |
| CN108624319A (en) * | 2018-05-31 | 2018-10-09 | 杭州电子科技大学 | A kind of white light LEDs borate orange fluorescent powder and preparation method thereof |
| CN108624319B (en) * | 2018-05-31 | 2021-03-23 | 杭州电子科技大学 | Borate orange fluorescent powder for white light LED and preparation method thereof |
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Application publication date: 20100901 |