CN101280458A - Growing method of carbon-doped sapphire crystal by EFG method - Google Patents

Growing method of carbon-doped sapphire crystal by EFG method Download PDF

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CN101280458A
CN101280458A CNA2007101737015A CN200710173701A CN101280458A CN 101280458 A CN101280458 A CN 101280458A CN A2007101737015 A CNA2007101737015 A CN A2007101737015A CN 200710173701 A CN200710173701 A CN 200710173701A CN 101280458 A CN101280458 A CN 101280458A
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crystal
carbon
growth
guided mode
sapphire crystal
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CN100575566C (en
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杨新波
徐军
李红军
程艳
赵广军
周国清
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Shanghai Institute of Optics and Fine Mechanics of CAS
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Abstract

Disclosed is a growth method of carbon-doped sapphire crystal through a guided mode method, which is characterized in that the guide mode method and a molybdenum-die are adopted for the growth of Alpha-Al2O3:C crystals. The alumina block with a certain weight through the high temperature sintering is disposed in a crucible of the molybdenum guided mode die, loaded inside a pulling furnace that is in vacuum-pumping to 10<-3> to 10<-4>Pa. Through the resistance heating, the temperature is continuously increased to 2050 to 2100 DEG C and then in constant temperature for 0.5 to 1 hour. Afterwards, the seed crystals are used for the growth of Alpha-Al2O3:C crystals. The Alpha-Al2O3:C crystals obtained from the growth are disposed in an annealing furnace of 1000 to 1500 DEG C under an atmosphere of hydrogen to preserve the heat for 50 to 100 hours. With the invention, the Alpha-Al2O3:C crystals with excellent thermoluminescence and optically stimulated luminescence properties can rapidly grow. Therefore, the invention can be applied in the manufacturing of highly sensitive thermoluminescence and optically stimulated luminescence detector.

Description

The method of growing method of carbon-doped sapphire crystal by EFG
Technical field
The present invention relates to carbon-doped sapphire crystal and (be designated hereinafter simply as α-Al2O3:C), particularly a kind of method of growing method of carbon-doped sapphire crystal by EFG, α-Al 2O 3: the C crystal is mainly for the manufacture of thermoluminescence and photoluminescent detector.
Background technology
Nineteen ninety, M.S.Akselrod professor reported first α-Al 2O 3: the C crystal also finds that it has very excellent thermoluminescence (Thermoluminescent is called for short TL) performance (M.S.Akselrod et.al.Highly sensitive thermoluminescent anion-defective α-Al 2O 3: C single crystaldetectors, Radiation Protection Dosimetry, 1990,32:15-20).α-Al 2O 3: C crystallo-luminescence peak temperature is about 187 ℃, and being subjected to thermoluminescent peak wavelength behind the irradiation is 420nm, and thermoluminescence sensitivity is LiF:Mg, 40～60 times of Ti, and the background threshold dose only is 10 -6Gy, its dose response is linearity-sublinear, linearity range is 10 -6～10Gy.α-Al 2O 3: the thermoluminescence performance of C crystal mainly is that Vo ¨ captures two electronics and generates the F colour center because the F colour center that exists in the crystal causes that it derives from causing of C and causes oxygen ion vacancy defective Vo ¨.Nineteen ninety-five, B.G.Markey etc. have studied α-Al first 2O 3: the light of C crystal is released light (Optical Stimulated Luminescence is called for short OSL) performance (B.G.Markey et.al.Time-resolved optical stimulated luminescence from α-Al 2O 3: C, RadiationMeasurements, 1995,24:457), find α-Al 2O 3: the glow peak of C crystal is positioned at 410nm, causes owing to the F colour center equally.α-Al 2O 3: the C crystal is used to make thermoluminescent detector (TLD) and has lot of advantages, and for example thermoluminescence is highly sensitive, is thermoluminescence crystal LiF:Mg, 40～60 times of Ti; Near 187 ℃ glow peak type is single, effective atomic number relatively low (10.2); Low predose response threshold value, the background threshold dose only is 10 -6Gy; The radiation dose response is linearity-sublinear, and linear response range is wide, 10 -6～10Gy; α-Al 2O 3: the emission peak at C crystal 4 20nm place is in (the M.S.Akselrod et.al.Preparation and Properties of α-Al such as best peak value of photomultiplier response 2O 3: C, RadiationProtection Dosimetry, 1993,47:159-164).
The guided mode method claims again edge limited-film feed (Edge-Defined, Film-Fed Growth are called for short EFG) method is mainly used in the crystal of growth specified shape, and in fact it is a kind of distortion of crystal pulling method.The characteristics of guided mode method growing crystal be can direct growth different shape (sheet, band shape, tubulose, fiber etc.) crystal, fast growth, crystalline size can accurately be controlled, and simplify the crystalline work program, reduce production costs.α-Al that M.S.Akselrod uses 2O 3: the C crystal is under the condition that has graphite to exist, (M.S.Akselrod et.al.Highly sensitive thermoluminescent anion-defective α-Al that φ 5 * 500mm sapphire crystal is annealed under strongly reducing atmosphere and obtained 2O 3: C single crystaldetectors, Radiation Protection Dosimetry, 1990,32:15-20).This method prerequisite is the bar-shaped sapphire crystal of growth high-quality, and then reduced anneal, the technology relative complex, and be difficult to guarantee the even distribution of carbon in sapphire crystal, namely be difficult to obtain the α-Al of quality homogeneous 2O 3: the C crystal.
Summary of the invention
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art, a kind of method of growing method of carbon-doped sapphire crystal by EFG is provided, this method can Fast Growth α-Al 2O 3: the C crystal.
Technical solution of the present invention is:
A kind of method of growing method of carbon-doped sapphire crystal by EFG is characterized in adopting guided mode method growth α-Al 2O 3: the C crystal, utilize the carbon in graphite heater and the graphite heat-insulation layer in growth course, to enter sapphire crystal, reach the purpose of carbon dope, adopt then the hydrogen high annealing, obtain having α-Al that good thermoluminescence and light are released optical property 2O 3: the C crystal.
The concrete technical process of the method for described growing method of carbon-doped sapphire crystal by EFG is as follows:
1. weigh 99.999% α of certain mass-Al 2O 3Powder was cold-pressed into bulk, 1300～1800 ℃ high temperature sinterings 24 hours;
2. with the α-Al that sinters 2O 3Block is packed in the molybdenum system crucible with guided mode mould, in the lifting furnace of packing into, lifting furnace is evacuated to 1 * 10 -3～1 * 10 -4Pa, resistive heating is persistently overheating to 2050～2100 ℃, constant temperature 0.5～1 hour;
3. oriented seed is slowly put down, make it to contact with the melt liquid level at the guided mode mould top of molybdenum system, keep temperature stable, treat α-Al 2O 3Melt launches at the die tip uniform spreading, starts the shift mechanism grown crystal after several minutes, and growth rate is 5～50mm/h;
4. slow cooling is to room temperature, takes out crystal and places under the hydrogen atmosphere 1000～1500 ℃ annealing furnace to be incubated 50～100 hours, obtains α-Al 2O 3: the C crystal;
Adopt graphite resistance heating and graphite thermal insulation layer to control the temperature field.
The carbon-doped sapphire crystal that obtains is used for the manufacturing of thermoluminescence and photoluminescent detector.
Technique effect of the present invention:
Prepare α-Al with M.S.Akselrod 2O 3: the method for C crystal is compared, and the present invention adopts the grow fast α-Al of various shapes of guided mode method 2O 3: the C crystal, the manufacturing procedure of crystal can effectively be saved cost when having simplified later stage manufacturing thermoluminescence and photoluminescent detector.Experimental result shows, the α-Al of guided mode method Fast Growth 2O 3: the C crystal has good thermoluminescence behind the hydrogen high annealing and light is released optical property, and crystal mass is good, can be for the manufacture of highly sensitive thermoluminescence and photoluminescent detector.
Description of drawings
Fig. 1 is guided mode method growth sheet α-Al of the present invention 2O 3: the molybdenum that adopts during C crystal crucible processed and die drawing
Fig. 2 is guided mode method growth α-Al of the present invention 2O 3: the thermoluminescence dose of radiation response curve of C crystal
Fig. 3 is guided mode method growth α-Al of the present invention 2O 3: the light of C crystal is released the light radiation dose response curve
Fig. 4 is growth tubulose α-Al 2O 3: the molybdenum that adopts during C crystal crucible processed and guided mode mould schematic diagram
Fig. 5 is the bar-shaped α-Al of growth 2O 3: the molybdenum that adopts during C crystal crucible processed and guided mode mould schematic diagram
Among the figure: 1-top cover, 2-crucible, 3-guided mode, 4-tubule, 5-guided mode tubule top cross-section
Embodiment
The invention will be further described below by embodiment, but should not limit protection scope of the present invention with this.
Embodiment 1: sheet α-Al 2O 3: the preparation of C crystal
Weigh 500 gram 99.999% α-Al 2O 3, under 200MPa, be cold-pressed into columned block, then 1500 ℃ of sintering 24 hours in the Si-Mo rod high temperature furnace.Fig. 1 is the present invention sheet α-Al that grows 2O 3: molybdenum crucible processed and mould schematic diagram that the C crystal is used.Open top cover 1 with the α-Al that sinters 2O 3Block is packed in the crucible 2, in the lifting furnace of packing into.Lifting furnace is evacuated to 5 * 10 -3Pa, graphite resistance is heating and continuous to be warming up to 2080 ℃, constant temperature 0.5 hour; The temperature at control guided mode 3 tops makes it a little more than the crystalline fusing point, then
Figure A20071017370100051
The direction seed crystal puts down, and makes it to contact with the melt liquid level at guided mode mould 3 tops, notes observing the fusing of seed end.Melt in seed end and the tubule 4 slowly fuses into one, start shift mechanism after several minutes, because the effect of melt and newborn crystalline avidity and smelt surface tension, the melt in the tubule will launch in mould top cross-section 5, until whole coverings, the growth velocity of employing is 30mm/h.Crystal growth finishes, and takes out crystal, puts it in the hydrogen annealing furnace, and insulation is 80 hours in lower 1300 ℃ of the hydrogen atmosphere, is cooled to room temperature, obtains α-Al 2O 3: the C crystal;
Utilize the sheet α of the inventive method growth-Al 2O 3: the C crystal perfection, no obvious wrappage is gentle behind the hydrogen annealing bubbles out now.Along r
Figure A20071017370100061
Direction is cut the sheet of 5 * 5 * 1mm in crystal, detect its thermoluminescence Characteristics and dose response curve thereof.α-Al behind the hydrogen annealing 2O 3: the C crystal shows the α-Al of guided mode method growth through the three-dimensional Thermo-luminescence of X-ray irradiation after 10 seconds 2O 3: the glow peak of C crystal is positioned at 190 ℃ to be located, and the peak type is single, and the thermoluminescence luminous intensity reaches 1.21 * 10 when 463K 4Cps, its emission wavelength is positioned at 415nm.Measuring result as shown in Figures 2 and 3.Fig. 2 is the α-Al of guided mode method growth of the present invention 2O 3: C crystalline thermoluminescence radiation dose response curve, 5 * 10 -6In～1Gy (gray(Gy)) the radiation dose scope, crystalline thermoluminescence intensity and radiation dose are good linear relationship.Fig. 3 is the α-Al of guided mode method growth 2O 3: the light of C crystal is released the light radiation dose response curve, and light releases luminous intensity and dose of radiation is linear, and luminous intensity strengthens along with the increase of dose of radiation.In a word, the α-Al of guided mode method growth 2O 3: thermoluminescence and the light α-Al that release optical property and M.S.Akselrod report of C crystal behind hydrogen annealing 2O 3: the C crystal property is suitable.
Embodiment 2: difform α-Al grows 2O 3: the C crystal
At α-Al 2O 3: in the C crystal application process, may concrete requirement be arranged to crystal shape,, tubulose bar-shaped such as needs, fibrous etc.The characteristics that the guided mode method is the most outstanding are exactly can grow to have the crystal of special shape, and the shape of crystal is controlled by the cross section of designing different guided mode moulds top.Growth tubulose and bar-shaped α-Al 2O 3: the crucible schematic diagram with guided mode mould of C crystal design as shown in Figure 4 and Figure 5, the growth technique of crystal is with embodiment 1.The crystal that growth is finished is annealed under the high-temperature hydrogen condition, obtain having α-Al that good thermoluminescence and light are released optical property 2O 3: the C crystal.
Embodiment 3: the α-Al that obtains under the different hydrogen annealing temperature 2O 3: the C crystal
α-Al that the growth of guided mode method obtains 2O 3: under hydrogen atmosphere 1000 ℃ respectively in C crystal, 1250 ℃, insulation is 80 hours in 1500 ℃.Found that the crystal under the different temperatures behind the hydrogen annealing all has thermoluminescence and light is released light characteristic, just thermoluminescence and light are released light intensity and changed to some extent under the irradiation same dose, and is mainly relevant with the F colour center that exists in the crystal.Along with the raising of hydrogen annealing temperature, increase gradually in the oxygen room in the crystal, and the F colour center defective that causes existing in the crystal increases, so α-Al 2O 3: glow peak that the C crystal is 190 ℃ strengthens, 1000 ℃ of recording in 10 seconds of x-ray irradiation, and 1250 ℃, the crystal after 1500 ℃ of annealing is positioned at 190 ℃ of glow peak intensity of locating and is respectively 2300cps, 6700cps, 16870cps, intensity differs greatly.
Embodiment 4: α-Al 2O 3Powder high temperature sintering temperature is to α-Al 2O 3: the impact of C crystal property
With high-purity α-Al 2O 3Powder is cold-pressed into bulk, respectively 1300,1500, and 1800 ℃ of sintering 24 hours, the growth technique of crystal is with embodiment 1.Found that α-Al that the powder under the different sintering temperatures obtains under isometric growth technology 2O 3: it is suitable that the thermoluminescence of C crystal and light are released optical property, and sintering temperature is more high, and the powder of putting in crucible is more many, and the crystal of growth is more big, the cost relative reduce.
Embodiment 5: lifting furnace vacuum is to α-Al 2O 3: the impact of C crystal property
The vacuum tightness of lifting furnace is evacuated to 1 * 10 respectively -3, 5 * 10 -3, 1 * 10 -4Pa, the crystalline growth technique is with embodiment 1.Found that, along with the raising of lifting furnace vacuum, α-Al that growth obtains 2O 3: the thermoluminescence of C crystal and light are released luminous sensitivity and are improved gradually, mainly are because the oxygen room difference that exists in the crystal causes.
Embodiment 6: resistance heated intensification temperature and constant temperature time are to α-Al 2O 3: the impact of C crystal property
The graphite resistance heat temperature raising is respectively to 2050,2075, and 2100 ℃, constant temperature 0.5 and 1 hour then, the crystalline growth technique is with embodiment 1.Found that the temperature of resistance heated and constant temperature time are to α-Al 2O 3: it is little that the thermoluminescence of C crystal and light are released the optical property impact.
Embodiment 7: growth rate is to α-Al 2O 3: the impact of C crystal property
Adopting the rate of pulling in the process of growth respectively is 5,25,50mm/h, and other growth techniques of crystalline are with embodiment 1.Found that the crystal that different growth velocitys obtain all has thermoluminescence behind hydrogen annealing and light is released optical property.Along with the raising of crystal growth rate, α-Al 2O 3: the thermoluminescence of C crystal and light are released optical property and are reduced, but production efficiency improves gradually.

Claims (4)

1, a kind of method of growing method of carbon-doped sapphire crystal by EFG is characterized in that adopting guided mode method growth α-Al 2O 3: the C crystal, utilize the carbon in graphite heater and the graphite heat-insulation layer in growth course, to enter sapphire crystal, reach the purpose of carbon dope, then high annealing in hydrogen atmosphere.
2, the method for growing method of carbon-doped sapphire crystal by EFG according to claim 1 is characterized in that the concrete technical process of this method is as follows:
1. weigh 99.999% α of certain mass-Al 2O 3Powder was cold-pressed into bulk, 1300～1800 ℃ high temperature sinterings 24 hours;
2. with the α-Al that sinters 2O 3Block is packed in the molybdenum system crucible with guided mode mould, in the lifting furnace of packing into, lifting furnace is evacuated to 1 * 10 -3～1 * 10 -4Pa, resistive heating is persistently overheating to 2050～2100 ℃, constant temperature 0.5～1 hour;
3. oriented seed is slowly put down, make it to contact with the melt liquid level at the guided mode mould top of molybdenum system, keep temperature stable, treat α-Al 2O 3Melt launches at the die tip uniform spreading, starts the shift mechanism grown crystal after several minutes, and growth rate is 5～50mm/h;
4. slow cooling is to room temperature, takes out crystal and places under the hydrogen atmosphere 1000～1500 ℃ annealing furnace to be incubated 50～100 hours, obtains α-Al 2O 3: the C crystal.
3, the method for growing method of carbon-doped sapphire crystal by EFG according to claim 1 is characterized in that adopting graphite resistance heating and graphite heat-insulation layer to control the temperature field.
4, the method for growing method of carbon-doped sapphire crystal by EFG according to claim 1 is characterized in that the carbon-doped sapphire crystal that is obtained is used for the manufacturing of thermoluminescence and photoluminescent detector.
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CN105862128A (en) * 2016-06-03 2016-08-17 景德镇陶瓷大学 Preparation method of normal-temperature high-strength mechanical property aluminum oxide wafer suitable for screen material and product prepared by same
CN106801254A (en) * 2017-01-22 2017-06-06 山东大学 A kind of CsSrI3The preparation method of scintillation crystal
CN106801254B (en) * 2017-01-22 2019-10-01 山东大学 A kind of CsSrI3The preparation method of scintillation crystal
CN110230095A (en) * 2019-05-21 2019-09-13 南京同溧晶体材料研究院有限公司 Device and method is used in a kind of rodlike colour jewel growth
CN111549374A (en) * 2020-06-19 2020-08-18 北方民族大学 Growing (near) stoichiometric lithium tantalate (LiTaO) by guided mode method3) Method for producing crystals

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