CN101603204B - Thermoluminescent or photoluminescent dosimetry crystal and preparation method thereof - Google Patents
Thermoluminescent or photoluminescent dosimetry crystal and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of laser crystal, in particular to a thermoluminescent or photoluminescent dosimetry crystal and a preparation method thereof. The thermoluminescent or photoluminescent dosimetry crystal is a carbon-doped yttrium aluminium garnet crystal. The invention also discloses a preparation method of the crystal, comprising the following steps: processing the raw materials by techniques of mixing, grinding and forming according to the proportion and preparing crystal growing material and then adopting a guiding temperature gradient method or a descending method for growing crystal in a reducing atmosphere. The carbon-doped yttrium aluminium garnet crystal has the advantages of higher thermoluminescent and photoluminescent sensibility, wider linear dosage response range and better thermoluminescent and photoluminescent stability, and simultaneously has the advantages of convenient processing, low temperature for crystal growing and lower cost.
Description
Technical field
The invention belongs to the laser crystals field, be specifically related to a kind of thermoluminescence or light and release dosimetry crystal and preparation method thereof.
Background technology
The thermoluminescence of material (Thermoluminescence is called for short TL) is meant the thermoluminescence of material after absorbed radiation energy.The 1950's; The Daniels of Univ Wisconsin-Madison USA is used for the thermoluminescence Characteristics of material the measurement (F.Daniels of radiation dose first; Thermoluminescence dosimetry seminar on the effects of ionizing radiations; Evans Signal Corps Engineering Laboratories, Belmar, N.J.1953).Up to the present, the thermoluminescent dosimetry material that comes into operation mainly contain LiF series (LiF:Mg, Ti and LiF:Mg, Cu, P), BeO series (BeO:Li, BeO:Na, BeO:Al), CaSO
4Series (CaSO
4: Mn, CaSO
4: Tm, CaSO
4: Dy), CaF
2Series (CaF
2: Mn, CaF
2: Dy, CaF
2: Tm) and Li
2B
4O
7Series (Li
2B
4O
7: Mn, Li
2B
4O
7: Cu, Ag).
Yet above-mentioned materials all more or less exists not enough on thermoluminescent dosimetry, can not satisfy scientific research and commercial needs.For example, lithium fluoride series is used the most extensive at present, and the thermoluminescence excellent property exists with powder type but its main drawback is a material, is not easy to processing and annealing; The thermoluminescence of calcium sulfate series is highly sensitive, but the main glow peak temperature is on the low side, and the thermoluminescence signal degradation is serious; The thermoluminescence sensitivity of Calcium Fluoride (Fluorspan) series is higher, but photic decline is very serious; The thermoluminescence peak of lithium tetraborate series is single and temperature is moderate (200 ℃), and shortcoming is that store heat photoluminescence signal capabilities is relatively poor, and sensitivity is not high.
Light is released light (Optically Stimulated Luminescence; Be called for short OSL) pl-after the radiating capacity that has been meant absorbed; The Romanovsky of the FSU releases measurement (the V.V.Romanovsky et al.Conference of the Academy of Sciences of the USSR on the Peaceful Uses ofAtomic Energy that light characteristic is used for radiation dose with the light of material the earliest; 1955, MOSCOW).Compare with thermoluminescence, light is released in the Fluorescent Densitomet use and need not be heated, and can effectively avoid the thermal quenching of luminescence center, has highly sensitively, uses simple relatively advantage.Yet light releases that the light dosage schoolmate phase does not obtain paying attention to and development, and major cause is to lack that radiation-sensitive, light are released the optical efficiency height, effective atomic number is less, it is good that light decay moves back performance light is released luminescent material.
In sum, the luminescent material of releasing thermoluminescence that uses at present or light has seriously hindered thermoluminescence or light and has released the development that light dosage is learned.Therefore, the thermoluminescence of exploitation high comprehensive performance or light are released luminescent material has become those skilled in the art institute problem demanding prompt solution.
The nineties in 20th century, people such as Akselrod have adopted Czochralski grown a kind of good Al
2O
3Doping thermoluminescence material α-Al
2O
3: C crystal (M.S.Akselrod, et al.1990 Radiat.Prot.Dosim.32,15).A series of research shows, α-Al
2O
3: the C crystal has highly sensitive (be LiF:Mg under the same terms, the 40-60 of Ti is doubly), thermal glow peak single (463K), and the back of the body end and dosage threshold value are low, linear dose response wide ranges (10
-7-10Gy), and effective atomic number little (10.2), thermoluminescence Characteristics decay slow (rate of fall-off is lower than 5%/a), repeat performance is good under the low dosage, and radiation-sensitive, light are released plurality of advantages such as optical efficiency height.YAG crystalline mineral name is the carbon-doped yttrium aluminium garnet, and molecular formula is Y
3Al
5O
12The YAG crystal has good materialization and optical property, is crucial substrate material in the laser crystals.Recently, Rodriguez etc. have reported that in succession YAG and nanocrystalline thermoluminescence or the light of doping YAG releases optical property (R.A.Rodr ì guez, et al.2004 Opt.Mater.27,293; R.A.Rodr ì guez, et al.2005 J.Phys.D Appl.Phys.38,3854; De la Rosa, et al.2005 Opt.Mater.27,1245).Discover, under the β x ray irradiation x, pure YAG and Tb
3+, Ce
3+, Er
3+, yb
3+Doped YAG is nanocrystalline to have very high thermoluminescence or light is released luminous sensitivity, and releasing light dosage field at thermoluminescence or light has potential using value.Yet, above-mentioned YAG nanocrystalline thermoluminescence or light release light property dose response and stable aspect also have tangible deficiency; Simultaneously, existing α-Al
2O
3: C crystalline growth temperature is very high, therefore causes production cost higher.
Summary of the invention
The object of the present invention is to provide a kind of thermoluminescence or light to release dosimetry crystal and preparation method thereof.
To achieve these goals, the technical scheme of the present invention's employing is following:
A kind of thermoluminescence or light are released dosimetry crystal, and this crystal is a kind of carbon-doped yttrium aluminium garnet (YAG:C) crystal.
Preferably, the doping of carbon is 10～20000ppm of crystal total mass in said carbon-doped yttrium aluminium garnet (YAG:C) crystal.
Preferred, the doping of carbon is 2000～8000ppm of crystal total mass in the said carbon-doped yttrium aluminium garnet crystal.
The preparation method that thermoluminescence of the present invention or light are released dosimetry crystal comprises the steps:
By proportioning raw material is made the crystal growth raw material through batch mixing, grinding and moulding process, adopt warm terraced method of guiding or descent method in reducing atmosphere, to grow then and make.
Said raw material comprises: contain Al element raw material, contain the Y element raw material and contain C element raw material.
Preferably, the said Al of containing element raw material is α-Al
2O
3Containing the Y element raw material is Y
2O
3Contain C element raw material and be selected from carbon dust or graphite.
The said Al of containing element raw material, contain the Y element raw material and contain C element proportion of raw materials and can calculate by the doping content of carbon in the mol ratio of YAG crystal Al and Y and the crystal.
Preferably, said moulding process is a cold isostatic compaction.
Preferably, said reducing atmosphere is a hydrogen atmosphere.
Preferably, the concrete steps of the terraced method growing crystal of said guiding temperature are: in crucible, put into seed crystal, the crystal growth raw material is put into crucible; Crucible is packed in the crystal furnace, be evacuated to furnace pressure＜5 * 10
-3Pa, persistently overheating to 2253～2283K, treat raw material fusing back constant temperature 0.5～2h, then with the speed cooling growing crystal of 1～5K/h.
Preferably, said crucible is a sealed crucible, more preferably seals the molybdenum crucible.
Preferably, said seed crystal is (001) direction YAG crystal.
Preferably, said descent method for growing crystalline concrete steps are: in crucible, put into seed crystal, the crystal growth raw material is put into crucible; Crucible is packed in the crystal furnace, be evacuated to furnace pressure＜5 * 10
-3Pa, persistently overheating to 2253～2283K, treat raw material fusing back constant temperature 0.5～2h, then with the speed decline crucible growing crystal of 0.5～3mm/h.
Preferably, said crucible is a sealed crucible, more preferably seals the molybdenum crucible.
Preferably, in the above-mentioned descent method for growing crystalline process, the growth interface thermograde is: 30～40K/cm.
The invention provides a kind of thermoluminescence or light and release dosimetry crystal; This crystal mixes certain mass fractional carbon dust or graphite in the YAG crystal; Adopt warm terraced method of guiding or descent method in reducing atmosphere, to grow and obtain the YAG:C crystal, wherein the doping of carbon is 10～20000ppm in this carbon-doped yttrium aluminium garnet crystal.Introducing and reducing atmosphere growth down through carbon; In the YAG crystal, produce certain density oxygen room; Oxygen room trapped electron produces a large amount of colour centers, releases the deathnium and the trap level of photoreduction process for thermoluminescence or light, reaches to improve the purpose that YAG crystalline thermoluminescence or light are released optical property.The growth under reducing atmosphere of YAG crystal can produce colour center equally, and the introducing of carbon may improve the concentration of colour center in the crystal, optimizes the purpose that YAG crystal thermoluminescence or light are released light characteristic thereby reach.Compare with YAG and other doping YAG nanocrystal; Carbon dope YAG crystal of the present invention has higher thermoluminescence or light is released luminous sensitivity; Wideer linear dose response scope, better thermoluminescence or light are released the stability of optical property, have advantage easy to process simultaneously.With α-Al
2O
3: the C crystal is compared, and YAG:C crystal growth temperature of the present invention is lower, so cost reduces relatively.YAG:C crystal of the present invention is expected to be used for the manufacturing that thermoluminescence efficiently or light are released the light dosage detector.
Description of drawings
Fig. 1 used close crucible structural representation of YAG:C crystal of growing.
The YAG:C crystalline abosrption spectrogram that makes among Fig. 2 embodiment 1.
The YAG:C crystalline thermoluminescence graphic representation that makes among Fig. 3 embodiment 1.
The YAG:C crystalline light that makes among Fig. 4 embodiment 1 is released the optical attenuation graphic representation.
The YAG:C crystalline dose response in thermoluminescence dosimetry graphic representation that makes among Fig. 5 embodiment 1.
The YAG:C crystalline light that makes among Fig. 6 embodiment 1 is released the light dosage response curve.
Embodiment
Further set forth the present invention below in conjunction with embodiment.Should be understood that these embodiment only are used to explain the present invention, and unrestricted scope of the present invention.
Embodiment 1: the YAG:C crystal that warm terraced method Growth of Carbon Doped amount is 5000ppm
Weigh the i.e. 255 gram α-Al of 2.5mol respectively
2O
3, the i.e. 338.7 gram Y of 1.5mol
2O
3With 2.96 gram carbon dusts be 5000ppm, mixed grinding 24h on planetary ball mill, take out the back cold dry-pressing formed for the material piece subsequent use.
Use airtight molybdenum crucible as shown in Figure 1 under hydrogen atmosphere; Adopt warm terraced method growth YAG:C crystal; Concrete steps are: select for use the pure YAG of (001) direction to do seed crystal; Seed slot 2 places at crucible as shown in Figure 11 put into YAG seed crystal 3, and the material piece 4 that suppresses is evenly put into crucible, cover crucible cover 5; Shove charge is evacuated to furnace pressure＜5 * 10
-3Pa, persistently overheating to～2253K, treat raw material fusing back constant temperature 0.5h; Speed cooling melt with 2K/h begins slow crystallization by the seed crystal place, continues cooling till the complete crystallization of melt, and the speed with 50K/h cools to room temperature again, promptly makes the YAG:C crystal.
The YAG:C crystal perfection that growth obtains does not have gentle the bubbling out of obvious wrap and shows the slightly micro-Huang of crystal.The sheet of in crystal, cutting 5 * 5 * 1mm along (001) direction is released optical property to the absorption spectrum that polishes the back sample and thermoluminescence or light and has been done test.
Shown in test result such as Fig. 2-6, wherein Fig. 2 is the YAG:C crystalline abosrption spectrogram that makes in the present embodiment.Compare with pure YAG, four tangible absorption peaks are arranged in the YAG:C crystal, lay respectively at 235,255,298 and the 370nm place.Fig. 3 is a YAG:C crystalline thermoluminescence curve, irradiation dose 2Gy, temperature rise rate 2K/s.The YAG:C crystal has very strong thermoluminescence effect, and finding has four thermoluminescence glow peaks, lays respectively at 115 ℃, 200 ℃, 255 ℃ and 300 ℃ and locates, and it is the strongest to locate luminous intensity with 115 ℃ and 255 ℃ especially.Fig. 4 is that YAG:C crystalline light is released the optical attenuation curve, and irradiation dose 2Gy uses blue LED array wavelength 470 ± 30nm optical excitation.YAG:C crystalline light is released light and is presented typical two exponential attenuation, and its light is released luminous sensitivity and is higher than thermoluminescence.Fig. 5 and Fig. 6 are respectively that YAG:C crystalline dose response in thermoluminescence dosimetry graphic representation and light are released the light dosage response curve, and what wherein dose response in thermoluminescence dosimetry was got is 200 ℃ of integral areas of locating glow peak, and light is released the integral area that extinction curve is got in the light dosage response.Can find out that from Fig. 5 and Fig. 6 the YAG:C crystalline thermoluminescence of present embodiment preparation or light are released the light dosage response and presented very significantly linear feature, have wide application potential in the radiation dosimetry field.
Embodiment 2: the YAG:C crystal that warm terraced method Growth of Carbon Doped amount is 10ppm
Except that the carbon dust that adds is the 10ppm, other are prepared burden with embodiment 1.Mixed grinding 24h on planetary ball mill, cold dry-pressing formed subsequent use after taking out for expecting piece.
Use airtight molybdenum crucible as shown in Figure 1 under hydrogen atmosphere; Adopt warm terraced method growth YAG:C crystal; Concrete steps are: select for use the pure YAG of (001) direction to do seed crystal; Seed slot 2 places at crucible as shown in Figure 11 put into YAG seed crystal 3, and the material piece 4 that suppresses is evenly put into crucible, cover crucible cover 5; Shove charge is evacuated to furnace pressure＜5 * 10
-3Pa, persistently overheating to～2283K, treat raw material fusing back constant temperature 2h; Begin slow crystallization with 1K/h speed cooling melt by the seed crystal place, continue cooling till the complete crystallization of melt, the speed with 40K/h cools to room temperature again, opens bonnet, takes out crystal, promptly makes the YAG:C crystal.
The YAG:C crystal perfection that growth obtains; Not having gentle the bubbling out of obvious wrap shows; It is similar that crystalline thermoluminescence or light are released among light characteristic and the embodiment 1 crystal; But be positioned at 235,255,298 and 370nm place uptake factor reduce, the sensitivity that crystalline thermoluminescence or light are released light under the same terms reduces, thermoluminescence or light are released light and are had the dosage linear response equally.
Embodiment 3: warm terraced method growth graphite dopping amount is the YAG:C crystal of 8000ppm
Except that the carbon dust that adds is that other were prepared burden with embodiment 1 8000ppm was.Mixed grinding 24h on planetary ball mill, cold dry-pressing formed subsequent use after taking out for expecting piece.
Use airtight molybdenum crucible as shown in Figure 1 under hydrogen atmosphere; Adopt warm terraced method growth YAG:C crystal; Concrete steps are: select for use the pure YAG of (001) direction to do seed crystal; Seed slot 2 places at crucible as shown in Figure 11 put into YAG seed crystal 3, and the material piece 4 that suppresses is evenly put into crucible, cover crucible cover 5; Shove charge is evacuated to furnace pressure＜5 * 10
-3Pa, persistently overheating to～2273K, treat raw material fusing back constant temperature 2h; Begin slow crystallization with 5K/h speed cooling melt by the seed crystal place, continue cooling till the complete crystallization of melt, the speed with 70K/h cools to room temperature again, opens bonnet, takes out crystal, promptly makes the YAG:C crystal.
The YAG:C crystal perfection that growth obtains; Not having gentle the bubbling out of obvious wrap shows; Crystal exists and to be positioned at 235,255,298 and the absorption peak at 370nm place, and thermal glow peak lays respectively at 116 ℃, 205 ℃, 258 ℃ and 310 ℃ and locates, and it is the YAG:C crystal height of 10ppm than carbon doping that thermoluminescence or light are released luminous sensitivity; Light is released light curve and is presented two exponential attenuatioies equally, and thermoluminescence or light are released light and had linear dose response equally.
Embodiment 4: warm terraced method growth graphite dopping amount is the YAG:C crystal of 20000ppm
Except that the graphite that adds is 20000ppm is, other batchings and growth step are with embodiment 1.It is complete that growth obtains brilliant YAG:C body; Not having gentle the bubbling out of obvious wrap shows; Crystal exists and to be positioned at 235,255,298 and the absorption peak at 370nm place; Thermal glow peak lays respectively at 116 ℃, 205 ℃, 258 ℃ and 310 ℃ and locates, and light is released light curve and presented two exponential attenuatioies equally, and thermoluminescence or light are released light and had the dosage linear response equally.
Embodiment 5: descent method for growing graphite dopping amount is the YAG:C crystal of 5000ppm
Weigh the i.e. 255 gram α-Al of 2.5mol respectively
2O
3, the i.e. 338.7 gram Y of 1.5mol
2O
3With 2.96 gram carbon dusts be 5000ppm, mixed grinding 24h on planetary ball mill, it is cold dry-pressing formed subsequent use to take out the back.Adopt descent method for growing YAG:C crystal, concrete steps are: in crucible, put into seed crystal, the crystal growth raw material that mixes is put into crucible, cover crucible cover; Shove charge is evacuated to furnace pressure＜5 * 10
-3Pa, persistently overheating to 2253K, treat raw material fusing back constant temperature 0.5h; The growth interface thermograde is: 30K/cm; With the speed decline crucible of 0.5mm/h, continue to descend up to the complete crystallization of melt then, the speed cooling with 40K/h makes carbon-doped yttrium aluminium garnet crystal again.
Embodiment 6: descent method for growing graphite dopping amount is the YAG:C crystal of 5000ppm
Weigh the i.e. 255 gram α-Al of 2.5mol respectively
2O
3, the i.e. 338.7 gram Y of 1.5mol
2O
3With 2.96 gram carbon dusts be 5000ppm, mixed grinding 24h on planetary ball mill, it is cold dry-pressing formed subsequent use to take out the back.Adopt descent method for growing YAG:C crystal, concrete steps are: in crucible, put into seed crystal, the crystal growth raw material that mixes is put into crucible, cover crucible cover; Shove charge is evacuated to furnace pressure＜5 * 10
-3Pa, persistently overheating to 2253K, treat raw material fusing back constant temperature 2h, the growth interface thermograde is: 40K/cm, then with the speed decline crucible of 3mm/h, continue to descend up to the complete crystallization of melt, the speed cooling with 70K/h makes carbon-doped yttrium aluminium garnet crystal again.
Claims (6)
1. thermoluminescence or light are released light dosage and are learned carbon-doped yttrium aluminium garnet monocrystalline, it is characterized in that the doping of carbon is 2000～8000ppm of crystal total mass in the said carbon-doped yttrium aluminium garnet crystal.
2. thermoluminescence described in the claim 1 or light are released the preparation method that light dosage is learned carbon-doped yttrium aluminium garnet monocrystalline; Comprise the steps: raw material to be made the crystal growth raw material through batch mixing, grinding and moulding process, adopt warm terraced method of guiding or descent method in reducing atmosphere, to grow then and make by proportioning;
The concrete steps of the terraced method growing crystal of said guiding temperature are: in crucible, put into seed crystal, the crystal growth raw material is put into crucible; Crucible is packed in the crystal furnace, be evacuated to furnace pressure＜5 * 10
-3Pa, persistently overheating to 2253～2283K, treat crystal growth raw material fusing back constant temperature 0.5～2h, then with the speed cooling growing crystal of 1～5K/h;
Said descent method for growing crystalline concrete steps are: in crucible, put into seed crystal, the crystal growth raw material is put into crucible; Crucible is packed in the crystal furnace, be evacuated to furnace pressure＜5 * 10
-3Pa, persistently overheating to 2253～2283K, treat raw material fusing back constant temperature 0.5～2h, then with the speed decline crucible growing crystal of 0.5～3mm/h.
3. thermoluminescence or light are released the preparation method that light dosage is learned carbon-doped yttrium aluminium garnet monocrystalline described in claim 2, it is characterized in that said raw material comprises and contains Al element raw material, contains the Y element raw material and contain C element raw material.
4. thermoluminescence or light are released the preparation method that light dosage is learned carbon-doped yttrium aluminium garnet monocrystalline described in claim 3, it is characterized in that the said Al of containing element raw material is α-A1
2O
3The said Y element raw material that contains is Y
2O
3The said C of containing element raw material is selected from carbon dust or graphite.
5. thermoluminescence or light are released the preparation method that light dosage is learned carbon-doped yttrium aluminium garnet monocrystalline described in claim 2, it is characterized in that said reducing atmosphere is a hydrogen atmosphere.
6. thermoluminescence described in the claim 1 or light are released light dosage and are learned carbon-doped yttrium aluminium garnet monocrystalline is released light dosage field at thermoluminescence or light application.
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|---|---|---|---|---|
| CN1562880A (en) * | 2004-04-09 | 2005-01-12 | 东北大学 | Ammonium hydrogen coprecipitation method for preparing nano powder of yttrium aluminum garnet and transparent ceramics |
| CN101311373A (en) * | 2008-04-14 | 2008-11-26 | 山东大学 | Process for synthesizing YAG single crystal nano-powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562880A (en) * | 2004-04-09 | 2005-01-12 | 东北大学 | Ammonium hydrogen coprecipitation method for preparing nano powder of yttrium aluminum garnet and transparent ceramics |
| CN101311373A (en) * | 2008-04-14 | 2008-11-26 | 山东大学 | Process for synthesizing YAG single crystal nano-powder |
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| Title |
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| JP平6-275903A 1994.09.30 |
| JP昭62-56396A 1987.03.12 |
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