CN106149053A - A kind of method of EFG technique growth high sensitivity thermoluminescence carbon-doped sapphire crystal - Google Patents
A kind of method of EFG technique growth high sensitivity thermoluminescence carbon-doped sapphire crystal Download PDFInfo
- Publication number
- CN106149053A CN106149053A CN201510171336.9A CN201510171336A CN106149053A CN 106149053 A CN106149053 A CN 106149053A CN 201510171336 A CN201510171336 A CN 201510171336A CN 106149053 A CN106149053 A CN 106149053A
- Authority
- CN
- China
- Prior art keywords
- carbon
- crystal
- doped sapphire
- sapphire crystal
- raw material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The method that the invention provides a kind of EFG technique growth high sensitivity thermoluminescence carbon-doped sapphire crystal, including: 1) take Al2O3Powder and purity are at least up to briquetting after the carbon dust of 6N uniformly mixes, and obtain raw material block；2) raw material block is placed in the sealed crucible in guided mode stove, uses EFG technique growth to obtain carbon-doped sapphire crystal.The present invention use the high-purity carbon dust of 6N as doping carbon source, to a certain extent realize the controlled of doping, it is possible to the highly sensitive thermoluminescence performance α-Al that fast-growth doping is controlled2O3: C crystal.
Description
Technical field
The present invention relates to a kind of carbon-doped sapphire (α-Al2O3: C) growing method of crystal, be specifically related to a kind of high-quality,
Thermoluminescence sensitivity reaches the α-Al of 1 μ Gy2O3: the growing method of C crystal, it is belonging to technical field of crystal growth.
Background technology
Natural gemstone is the Al containing impurity2O3Crystal, after raying, has thermoluminescence (TL) and light to release the phenomenon of light (OSL).
Now, manual method can synthesize pure Al2O3Monocrystalline or the α-Al of incorporation desired content impurity2O3Crystal, to obtain specific heat
Learn and optical property .Summers is to α-Al2O3Summary made by thermoluminescence material.Due to technologic reason, develop in early days
Doped alpha-Al2O3Crystal, thermoluminescence sensitivity is low, limits its application in thermoluminescent dosimetry.The nineties in 20th century
Just Akselrod et al. is with particle Al2O3Crystal is that host material is developed into α-Al2O3: C monocrystalline, heating rate is 4 DEG C of s
Time, glow peak temperature is 190 DEG C, and thermoluminescence sensitivity is LiF:Mg, 50 60 times of Ti, and background threshold dose is only
0.1 μ Gy, has good repeatability, and its dose response is linear sublinear, and the range of linearity is at 300nGy to 10Gy, effectively
Atomic is only 11.3.Therefore, α-Al2O3: C becomes the thermoluminescence of great potential quality and light releases luminescent material.
At present, α-Al2O3: the growth of C crystal and the manufacture of radiacmeter are mainly monopolized by Landauer company of the U.S., these public affairs
α-the Al of department's development and production2O3: C thermoluminescent dosimeter final products are powder compacting, have thrown in European & American Market, extensively should
For environment and personal dose monitoring.The most relevant the most domestic α-Al2O3: the report of C crystal growth.
Summary of the invention
It is contemplated that fill up, existing open source literature there is no α-Al2O3: the technological gap of C crystal preparation method, the present invention carries
Having supplied a kind of to grow the method that thermoluminescence sensitivity reaches 1 μ Gy carbon-doped sapphire crystal, feature is to be directly added into former with high-purity carbon dust
Material is as carbon source.
The invention provides and a kind of grow the method that thermoluminescence sensitivity reaches 1 μ Gy carbon-doped sapphire crystal, including:
1) Al is taken2O3Powder and purity are at least up to briquetting after the carbon dust of 6N uniformly mixes, and obtain raw material block；
2) raw material block is placed in the sealed crucible in guided mode stove, uses EFG technique growth to obtain carbon-doped sapphire crystal.
It is preferred that the material of described crucible and mould is molybdenum.
It is preferred that Al2O3Powder purity is at least up to 4N.
It is preferred that phosphorus content is 0.3wt%-1wt%, preferably 0.5wt% in carbon-doped sapphire crystal.
It is preferred that described growing method of carbon-doped sapphire crystal by EFG includes:
First, sealed crucible described in evacuation is also passed through noble gas, then raw material block is heated to 2000-2200 DEG C so that it is become
For melt, melt diffuses to guided mode top by the capillary tube slit of guided mode；
Secondly, seed crystal is placed in guided mode top, with melt contacts, after seed end fusing and fusing into one with melt, lifts
Operation, after lifting, cooling obtains carbon-doped sapphire crystal.
It is preferred that be evacuated to 10-3～10-4Pa。
It is preferred that the argon that described noble gas is purity 99.99%.
It is preferred that raw material block is heated to 2000-2200 DEG C with the programming rate of 150-250 DEG C/h.
It is preferred that described seed crystal isDirection sapphire.
It is preferred that pull rate is 5-10mm/ hour in EFG technique growth course, preferably 7mm/ hour.
It is preferred that the cross sectional shape of carbon-doped sapphire crystal is determined by the shape and size of guided mode top capillary tube slit.
Beneficial effects of the present invention:
α-the Al prepared with other EFG technique2O3: C crystal is compared, and the present invention uses the high-purity carbon dust of 6N as doping carbon source, certain journey
The controlled of doping is realized, it is possible to the highly sensitive thermoluminescence performance α-Al that fast-growth doping is controlled on degree2O3: C crystal, can
Manufacturing for high-sensitive thermoluminescent detector (TLD), detector is 5mm × 5mm × 1mm, direction isPolishing crystal
Thin slice.
Accompanying drawing explanation
Fig. 1 shows the α-Al of EFG technique growth in the embodiment of the present invention 12O3: C crystallogram；
Fig. 2 shows the α-Al of EFG technique growth in the embodiment of the present invention 12O3: the detector photo of C crystal pro cessing；
Fig. 3 shows α-Al in the embodiment of the present invention 12O3: the detector detector crystal face XRD figure spectrum of C crystal pro cessing；
Fig. 4 shows the α-Al of EFG technique growth in the embodiment of the present invention 12O3: C crystal β ray low dosage (less than 10Gy) heat
Release light dosage response curve；
Fig. 5 shows the α-Al of EFG technique growth in the embodiment of the present invention 12O3: C crystal β ray low dosage (less than 10Gy) light
Release light dosage response curve.
Detailed description of the invention
The present invention is further illustrated, it should be appreciated that accompanying drawing and following embodiment are only below in conjunction with accompanying drawing and following embodiment
For the present invention is described, and the unrestricted present invention.
It is an object of the present invention to provide a kind of α-Al2O3: the growing method of C crystal, overcome the deficiencies in the prior art, it is achieved α-
Al2O3: the fast-growth of C crystal and doping controlled.
A kind of EFG technique growth high sensitivity thermoluminescence carbon-doped sapphire crystal method, feature be use EFG technique, crucible and
Mould is molybdenum product, utilizes carbon dust high-purity for 6N to mix raw material and reaches carbon dope purpose as carbon source, grows α-Al2O3: C is brilliant
Body.
Described method comprises the following specific steps that:
(1) Al of certain mass is taken2O3Powder and carbon dust, as raw material, are put into after pretreatment in the crucible of band mould and are sealed；
(2) 10 it are evacuated to-3～10-4Pa, is passed through noble gas, is heated to 2100 DEG C with the programming rate of 200 DEG C/h；
(3) seed crystal is slowly put down, be allowed to the melt liquid level with die top and contact, note observing the fusing of seed end.Seed crystal
Top slowly fuses into one with the melt in capillary tube, starts shift mechanism after several minutes, and pull rate is 7mm/h；
(4) take out crystal after being slowly dropped to room temperature after having grown, obtain α-Al2O3: C crystal, crystal section shape is by guided mode top
The profile in portion and size determine.
Described pretreatment is that mixing and ball milling was cold-pressed into bulk after 24 hours, the block stock pressed cold through 300Mpa again
Isostatic pressed.
Described material purity Al2O3Powder be the carbon dust of 4N sum be 6N.
Described noble gas is the argon of 99.99%.
Described crucible and mould are molybdenum matter.
Described seed crystal isDirection sapphire.
The detector of described making is 5mm × 5mm × 1mm, direction isPolishing crystal microchip.
The method that the invention provides a kind of EFG technique growth high sensitivity thermoluminescence carbon-doped sapphire crystal, feature is to use
EFG technique, crucible and mould are molybdenum product, grow α-Al2O3: C crystal.By the Al of purity 4N2O3The carbon dust of powder and 6N is made
For raw material, after mix homogeneously first pressing under 300MPa cold isostatic compaction, be then placed in the crucible of guided mode mould of molybdenum, dress
Entering in lifting furnace, will be filled with argon as protective gas after reverse mould stove evacuation, resistance is heating and continuous is warming up to 2100 DEG C, so
Tailing edgeDirection growth carbon-doped sapphire crystal (α-Al2O3: C crystal).The present invention can fast-growth doping controlled
Highly sensitive thermoluminescence performance α-Al2O3: C crystal, manufacture for high-sensitive thermoluminescent detector (TLD), detector is
5mm × 5mm × 1mm, direction arePolishing crystal microchip.
The technique effect of the present invention:
α-the Al prepared with other EFG technique2O3: C crystal is compared, and the present invention uses the high-purity carbon dust of 6N as doping carbon source, certain journey
The controlled of doping is realized, it is possible to the highly sensitive thermoluminescence performance α-Al that fast-growth doping is controlled on degree2O3: C crystal, can
Manufacturing for high-sensitive thermoluminescent detector (TLD), detector is 5mm × 5mm × 1mm, direction isPolishing crystal
Thin slice.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following example are served only for this
Bright it is further described, it is impossible to being interpreted as limiting the scope of the invention, those skilled in the art is according to the present invention's
Some nonessential improvement and adjustment that foregoing is made belong to protection scope of the present invention.The technique ginseng that following example is concrete
Number etc. is the most only an example in OK range, in the range of i.e. those skilled in the art can be done suitably by explanation herein
Select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
Use molybdenum molding jig and crucible, with high-purity 2487.5g Al2O3Powder and 12.5g graphite powder are raw material, after mix homogeneously
Under 300MPa cold isostatic compaction and under 1.08 atmospheric pressure argon gas atmosphere in guided mode stove grow crystal, raw material shove charge is complete
After, start heating power supply, be heated to 2100 DEG C with the programming rate of 200 DEG C/h, then willDirection sapphire seed crystal
Slowly put down, be allowed to the melt liquid level with die top and contact, note observing the fusing of seed end.Seed crystal top and capillary tube
In melt slowly fuse into one, start shift mechanism after several minutes, pull rate is 7mm/h.Due to melt and nascent crystals
Affinity and the effect of smelt surface tension, the melt in capillary tube will launch at die top, until all covering.With
The slow lifting of seed crystal, crystal growth is constantly carried out, until melt is exhausted, the crystal section shape grown is by guided mode top
The profile in portion and size determine, thermoluminescent detector (TLD) material is the α-Al2O3:C monocrystalline of EFG technique growth, inner circle cutting machine cut
A size of 5mm × 5mm × 1mm, the direction is become to beCrystal microchip, finally crystal microchip is done twin polishing process；
From figure 1 it appears that the wafer surface taken out from molybdenum crucible has small growth striation, draw mainly due to temperature field wave is dynamic
Rise.Having a small amount of atrament to be attached to wafer surface at wafer afterbody, XRD test shows that black attachment is mainly stone
Ink and MoC2, it is that in crystal growing process, the volatilization of high-purity carbon dust causes；
From figure 2 it can be seen that α-Al2O3: C crystal is faint yellow；
From figure 3, it can be seen that α-Al2O3: C crystal prototype diffraction maximum 2 θ is 37.6 °, for a face；
Figure 4, it is seen that α-Al2O3: C crystal β ray low dosage dose response in thermoluminescence dosimetry curve is linearly；
From figure 5 it can be seen that α-Al2O3: C crystal β ray low dosage optically stimulated luminescence dosage response curve is linearly.
Claims (10)
1. the method growing high sensitivity thermoluminescence carbon-doped sapphire crystal, it is characterised in that including:
1) Al is taken2O3Powder and purity are at least up to briquetting after the carbon dust of 6N uniformly mixes, and obtain raw material block；
2) raw material block is placed in the sealed crucible in guided mode stove, uses EFG technique growth to obtain carbon-doped sapphire crystal.
Method the most according to claim 1, it is characterised in that the material of described crucible and mould is molybdenum.
Method the most according to claim 1 and 2, it is characterised in that Al2O3Powder purity is at least up to 4N.
4. according to described method arbitrary in claim 1-3, it is characterised in that in carbon-doped sapphire crystal, phosphorus content is 0.3wt%-
1wt%, preferably 0.5wt%.
5. according to described preparation method arbitrary in claim 1-4, it is characterised in that described growing method of carbon-doped sapphire crystal by EFG
Including:
First, sealed crucible described in evacuation is also passed through noble gas, then raw material block is heated to 2000-2200 DEG C so that it is become
For melt, melt diffuses to guided mode top by the capillary tube slit of guided mode；
Secondly, seed crystal is placed in guided mode top, with melt contacts, after seed end fusing and fusing into one with melt, lifts
Operation, after lifting, cooling obtains carbon-doped sapphire crystal.
Preparation method the most according to claim 5, it is characterised in that be evacuated to 10-3～10-4Pa。
7. according to the preparation method described in claim 5 or 6, it is characterised in that described noble gas is the argon of purity 99.99%
Gas.
8. according to described preparation method arbitrary in claim 5-7, it is characterised in that by raw material block with 150-250 DEG C/h
Programming rate is heated to 2000-2200 DEG C.
9. according to described preparation method arbitrary in claim 5-8, it is characterised in that described seed crystal isDirection indigo plant is precious
Stone.
10. according to described preparation method arbitrary in claim 5-9, it is characterised in that in EFG technique growth course, pull rate is
5-10mm/ hour, preferably 7mm/ hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510171336.9A CN106149053A (en) | 2015-04-13 | 2015-04-13 | A kind of method of EFG technique growth high sensitivity thermoluminescence carbon-doped sapphire crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510171336.9A CN106149053A (en) | 2015-04-13 | 2015-04-13 | A kind of method of EFG technique growth high sensitivity thermoluminescence carbon-doped sapphire crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106149053A true CN106149053A (en) | 2016-11-23 |
Family
ID=57336604
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510171336.9A Pending CN106149053A (en) | 2015-04-13 | 2015-04-13 | A kind of method of EFG technique growth high sensitivity thermoluminescence carbon-doped sapphire crystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106149053A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107937983A (en) * | 2018-01-04 | 2018-04-20 | 河北工业大学 | A kind of sapphire material of multicomponent doping and its preparation method and application |
| CN111074337A (en) * | 2020-01-07 | 2020-04-28 | 同济大学 | Method and device for growing high-concentration titanium-doped sapphire crystals by guided mode method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101280458A (en) * | 2007-12-28 | 2008-10-08 | 中国科学院上海光学精密机械研究所 | Method for growing carbon-doped sapphire crystal by using guided mode method |
| CN102817072A (en) * | 2012-07-30 | 2012-12-12 | 鸿福晶体科技(安徽)有限公司 | Preparation method of doping raw material used for growing gem single crystal through edge-defined film-fed growth method |
| CN103014856A (en) * | 2013-01-10 | 2013-04-03 | 苏州巍迩光电科技有限公司 | Ferric-titanium-doped sapphire wafer and preparation method thereof |
-
2015
- 2015-04-13 CN CN201510171336.9A patent/CN106149053A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101280458A (en) * | 2007-12-28 | 2008-10-08 | 中国科学院上海光学精密机械研究所 | Method for growing carbon-doped sapphire crystal by using guided mode method |
| CN102817072A (en) * | 2012-07-30 | 2012-12-12 | 鸿福晶体科技(安徽)有限公司 | Preparation method of doping raw material used for growing gem single crystal through edge-defined film-fed growth method |
| CN103014856A (en) * | 2013-01-10 | 2013-04-03 | 苏州巍迩光电科技有限公司 | Ferric-titanium-doped sapphire wafer and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107937983A (en) * | 2018-01-04 | 2018-04-20 | 河北工业大学 | A kind of sapphire material of multicomponent doping and its preparation method and application |
| CN111074337A (en) * | 2020-01-07 | 2020-04-28 | 同济大学 | Method and device for growing high-concentration titanium-doped sapphire crystals by guided mode method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100575566C (en) | Method for growing carbon-doped sapphire crystal by using guided mode method | |
| JP5493092B2 (en) | Method for producing gallium oxide single crystal and gallium oxide single crystal | |
| CN108138359A (en) | Sic single crystal ingot | |
| WO2021004108A1 (en) | Neodymium-doped bgso mixed crystal material and preparation method therefor | |
| CN114524616B (en) | Lithium disilicate glass ceramic body with different light transmittance and preparation method thereof | |
| CN106149053A (en) | A kind of method of EFG technique growth high sensitivity thermoluminescence carbon-doped sapphire crystal | |
| CN114395802B (en) | Thallium-doped cesium iodide scintillation crystal preparation method and radiation detection panel | |
| TW202136599A (en) | Gallium arsenide crystalline body and gallium arsenide crystal substrate | |
| CN107354509A (en) | One kind mixes yttrium barium fluoride crystal and its preparation method and application | |
| WO2020078186A1 (en) | Fluorescent ceramic and preparation method therefor | |
| US3378431A (en) | Method of making carbon-containing glass and product thereof | |
| CN113213766B (en) | Perovskite quantum dot scintillation glass-ceramic and preparation method thereof | |
| CN1306075C (en) | Anion and cation co-doped PbWO4 crystal and its growth method | |
| Holovey et al. | X-ray induced optical absorption in Li2B4O7 and Li2B4O7: Cu single crystals and glasses | |
| CN105399334B (en) | One kind is embedded with GdTaO4Flicker devitrified glass of crystallite phase and preparation method thereof | |
| Asadov et al. | X-ray dosimetric characteristics of AgGaS 2 single crystals grown by chemical vapor transport | |
| CN101643936B (en) | Horizontal growth method for lead tungstate scintillation crystal | |
| CN115213403A (en) | Method for improving scintillation property of gallium oxide crystal with fast attenuation and high light output | |
| US11028016B2 (en) | Method of manufacture of copper-doped glasses | |
| US20100092363A1 (en) | Combustion synthesis method and materials produced therefrom | |
| CN115216840B (en) | Method for preparing lithium thallium co-doped sodium iodide scintillation crystal by ion compensation method | |
| US9523033B2 (en) | Method for large scale synthesis of optically stimulated luminescence grade polycrystalline ceramic material | |
| Iriqui Razcón et al. | Novel ZnO: Li phosphors for electronics and dosimetry applications | |
| CN111379025A (en) | Growth method of cesium-lead halide crystal | |
| US4217166A (en) | Process for the production of lithium fluoride detectors |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20161123 |