CN103409806A - Annealing method of neodymium, cerium and chromium doped yttrium aluminum garnet crystal - Google Patents
Annealing method of neodymium, cerium and chromium doped yttrium aluminum garnet crystal Download PDFInfo
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- CN103409806A CN103409806A CN2013103514106A CN201310351410A CN103409806A CN 103409806 A CN103409806 A CN 103409806A CN 2013103514106 A CN2013103514106 A CN 2013103514106A CN 201310351410 A CN201310351410 A CN 201310351410A CN 103409806 A CN103409806 A CN 103409806A
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- 239000013078 crystal Substances 0.000 title claims abstract description 83
- 239000011651 chromium Substances 0.000 title claims abstract description 71
- 238000000137 annealing Methods 0.000 title claims abstract description 44
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 24
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 24
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 22
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 title claims abstract description 14
- 229910052779 Neodymium Inorganic materials 0.000 title abstract 3
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 title abstract 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004917 carbon fiber Substances 0.000 claims abstract description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 claims description 26
- 238000010792 warming Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 9
- 230000006698 induction Effects 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 abstract description 10
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 229910052741 iridium Inorganic materials 0.000 abstract description 4
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 abstract description 4
- 230000003287 optical effect Effects 0.000 abstract description 4
- 239000010970 precious metal Substances 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 description 23
- 230000008859 change Effects 0.000 description 10
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 230000005945 translocation Effects 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses an annealing method of a neodymium, cerium and chromium doped yttrium aluminum garnet (YAG) crystal. The method comprises the steps that: a carbon fiber crucible is adopted; the neodymium, cerium and chromium doped yttrium aluminum garnet Nd<3+>:Ce<3+>:Cr<3+>:YAG crystal is placed into the crucible, and is embedded by using alumina powder; temperature and cleanness are maintained; an annealing furnace door is closed; high-purity argon is delivered into the furnace for protecting; the temperature is first increased to 400 DEG C with a speed of 100 DEG C/h, and is increased to 1200-1300 DEG C with a speed of 50-70 DEG C/h; the temperature is maintained for 12-36h; the temperature is reduced to 150-200 DEG C, and the power is shut off; the temperature is naturally reduced to 30 DEG C, and the crystal is fetched from the furnace. With the method, scattering particles and stress in the crystals are eliminated, such that crystal defect is reduced; crustal entire laser performance and optical performance are improved, and oxidation loss of a large amount of precious metal iridium is avoided.
Description
Technical field
The present invention relates to the thermal treatment process technology field of crystal, in particular yttrium aluminum garnet (the Nd of a kind of neodymium-doped, cerium and chromium
3+: Ce
3+: Cr
3+: the YAG) method for annealing of crystal.
Background technology
The yttrium aluminum garnet of neodymium-doped, cerium and chromium (is called for short Nd
3+: Ce
3+: Cr
3+: YAG) crystal annealing is some defects that produce in the crystal growth for eliminating, and removes by pyroprocessing, improves a kind of method of its optical homogeneity.Now general crystal annealing adopts other high temperature material crucibles such as retort furnace and ceramic crucible, and crystalline material is packed in crucible, and by heating up, constant temperature and temperature-fall period, anneal.
Nd
3+: Ce
3+: Cr
3+: YAG laser crystals, Nd
3+The main excited ion that activates laser in crystal, Ce
3+It is the sensitized ions in crystal.Ce
3+, Cr
3+Ion plays the auxiliary crystal energy that improves, doping Nd
3+Substitute the Y at dodecahedron center
3+, Ce
3+Also to substitute Y
3+, add simultaneously Ce
3+, Cr
3+The crystal growth is certain to occur serious lattice distortion, mixes Cr
3+Ion can play the effect of volume compensation, Cr
3+With substitute for Al
3+The mode lattice structure that enters crystal, therefore, serious lattice distortion can not occur in the crystal growth.
The Cr ion is substitute for Al in the YAG crystal
3+Ion has two kinds of coordinations: a kind of Cr
3+The Al of ionic replacement octahedral coordination
3+Ion position, a kind of Cr
4+The Al of ionic replacement tetrahedral coordination
3+Ion position.Cr in lattice
3+Ion is the most stable.Crystal is annealed in oxidizing atmosphere, can carry out compensation charge by two aspects: the one, produce oxygen vacancy, and the 2nd, a part of Cr ion becomes quadrivalent ion by trivalent, and enters tetrahedral site by unsettled octahedral site.
Other high temperature material crucible annealing such as retort furnace and ceramic crucible, carry out, therefore for Nd in reducing atmosphere
3+: Ce
3+: Cr
3+: the YAG crystal can not adopt.And adopt general crystal annealing method, often in crystal, cause a large amount of scattering particles, have certain growth stress, optics machining stress etc., had a strong impact on the laser activity of crystal.Adopt the Iridium Crucible Frequency Induction Heating, although in stove, the method for logical partial oxidation annealing can be eliminated scattering particles, also can cause the oxidation loss of a large amount of precious metal iridiums, and iridium is expensive, very expensive.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of scattering particles and the stress that can eliminate in crystal is provided, reduce lattice defect, improve whole laser activity and the optical property of crystal and avoided the method for annealing of yag crystal of neodymium-doped, cerium and the chromium of the oxidation loss of a large amount of precious metal iridiums.
The present invention is achieved by the following technical solutions:
The method for annealing of the yag crystal of a kind of neodymium-doped, cerium and chromium, comprise the steps:
(1) get carbon fiber crucible, put into the annealing furnace Frequency Induction Heating, then by the yttrium aluminum garnet Nd of neodymium-doped, cerium and chromium
3+: Ce
3+: Cr
3+: the YAG crystal is packed in crucible, uses the alumina powder landfill, does not allow Nd
3+: Ce
3+: Cr
3+: the YAG crystal exposes, and insulation, keep a public place clean;
(2) close door of annealing furnace, vacuumize, be filled with high-purity argon gas protection in annealing furnace;
(3) at first with the speed of 100 ℃/hour, be warming up to 400 ℃, then with the speed of 50-70 ℃/hour, be warming up to 1200-1300 ℃, constant temperature 12 hours-36 hours;
(4) with the speed of 5-20 ℃/hour, be cooled to 1000 ℃, then per hour than the cooling rate of falling 10-15 ℃ last hour, to be cooled to 150-200 ℃ more;
(5) powered-down, take out Nd while naturally being cooled to 30 ℃ in stove
3+: Ce
3+: Cr
3+: the YAG crystal.
As the preferred implementation of the method for annealing of the yag crystal of above-mentioned neodymium-doped, cerium and chromium, in described step (3), be constant temperature 24 hours at 1250 ℃ of temperature.
The present invention has the following advantages compared to existing technology:
The method for annealing of the yag crystal of a kind of neodymium-doped disclosed in this invention, cerium and chromium, eliminated the scattering particles that exist in the crystal, also eliminated growth stress, the optics machining stress equal stress of crystal, and Cr does not occur
3+Ion conversion becomes Cr
4+The ion translocation phenomenon, whole laser activity and the optics of raising crystal, improved its optical homogeneity.In addition, because this method for annealing adopts carbon fiber crucible and with alumina powder landfill crystal, both guaranteed to anneal in well-oxygenated environment, the oxidation loss problem of a large amount of precious metal iridiums that produced while having avoided again using Iridium Crucible toward the interior logical oxygen of stove, thus greatly saved cost.
Embodiment
Below embodiments of the invention are elaborated, the present embodiment is implemented take technical solution of the present invention under prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment mono-
The present embodiment is the preferred embodiments of the present invention, and the method for annealing of the yag crystal of the disclosed a kind of neodymium-doped of the present embodiment, cerium and chromium, comprise the steps:
(1) get carbon fiber crucible, put into the annealing furnace Frequency Induction Heating, annealing furnace can be used the monocrystalline stove, then by the yttrium aluminum garnet Nd of neodymium-doped, cerium and chromium
3+: Ce
3+: Cr
3+: the YAG crystal is packed in crucible, uses the alumina powder landfill, does not allow Nd
3+: Ce
3+: Cr
3+: the YAG crystal exposes, and insulation, keep a public place clean;
(2) close door of annealing furnace, vacuumize, be filled with high-purity argon gas protection in annealing furnace;
(3) at first with the speed of 100 ℃/hour, be warming up to 400 ℃, then with the speed of 50-70 ℃/hour, be warming up to 1250 ℃, constant temperature 24 hours;
(4) with the speed of 5-20 ℃/hour, be cooled to 1000 ℃, then per hour than the cooling rate of falling 15 ℃ last hour, to be cooled to 150-200 ℃ more;
(5) powered-down, take out Nd while naturally being cooled to 30 ℃ in stove
3+: Ce
3+: Cr
3+: the YAG crystal.
The crystal taken out is detected with 20 milliwatt green glows, and the scattering particles of crystal are eliminated fully.Then with the cross-polarized light stressometer, detect crystal stress basically eliminate.In addition, the crystal appearance color does not change, and shows Cr
3+Ion does not change into Cr
4+Ion.
Embodiment bis-
The method for annealing of the yag crystal of the disclosed a kind of neodymium-doped of the present embodiment, cerium and chromium, comprise the steps:
(1) get carbon fiber crucible, put into the annealing furnace Frequency Induction Heating, then by the yttrium aluminum garnet Nd of neodymium-doped, cerium and chromium
3+: Ce
3+: Cr
3+: the YAG crystal is packed in crucible, uses the alumina powder landfill, does not allow Nd
3+: Ce
3+: Cr
3+: the YAG crystal exposes, and insulation, keep a public place clean;
(2) close door of annealing furnace, vacuumize, be filled with high-purity argon gas protection in annealing furnace;
(3) at first with the speed of 100 ℃/hour, be warming up to 400 ℃, then with the speed of 50-70 ℃/hour, be warming up to 1300 ℃, constant temperature 24 hours;
(4) with the speed of 5-20 ℃/hour, be cooled to 1000 ℃, then per hour than the cooling rate of falling 10 ℃ last hour, to be cooled to 150-200 ℃ more;
(5) powered-down, take out Nd while naturally being cooled to 30 ℃ in stove
3+: Ce
3+: Cr
3+: the YAG crystal.
The crystal taken out is detected with 20 milliwatt green glows, and the scattering particles of crystal are eliminated fully.Then with the cross-polarized light stressometer, detect crystal stress basically eliminate.In addition, the crystal appearance color does not change, and shows Cr
3+Ion does not change into Cr
4+Ion.
Embodiment tri-
The method for annealing of the yag crystal of the disclosed a kind of neodymium-doped of the present embodiment, cerium and chromium, comprise the steps:
(1) get carbon fiber crucible, put into the annealing furnace Frequency Induction Heating, then by the yttrium aluminum garnet Nd of neodymium-doped, cerium and chromium
3+: Ce
3+: Cr
3+: the YAG crystal is packed in crucible, uses the alumina powder landfill, does not allow Nd
3+: Ce
3+: Cr
3+: the YAG crystal exposes, and insulation, keep a public place clean;
(2) close door of annealing furnace, vacuumize, be filled with high-purity argon gas protection in annealing furnace;
(3) at first with the speed of 100 ℃/hour, be warming up to 400 ℃, then with the speed of 50-70 ℃/hour, be warming up to 1300 ℃, constant temperature 36 hours;
(4) with the speed of 5-20 ℃/hour, be cooled to 1000 ℃, then per hour than the cooling rate of falling 15 ℃ last hour, to be cooled to 150-200 ℃ more;
(5) powered-down, take out Nd while naturally being cooled to 30 ℃ in stove
3+: Ce
3+: Cr
3+: the YAG crystal.
The crystal taken out is detected with 20 milliwatt green glows, and the scattering particles of crystal are eliminated fully.Then with the cross-polarized light stressometer, detect crystal stress basically eliminate.In addition, the crystal appearance color does not change, and shows Cr
3+Ion does not change into Cr
4+Ion.
Embodiment tetra-
The method for annealing of the yag crystal of the disclosed a kind of neodymium-doped of the present embodiment, cerium and chromium, comprise the steps:
(1) get carbon fiber crucible, put into the annealing furnace Frequency Induction Heating, then by the yttrium aluminum garnet Nd of neodymium-doped, cerium and chromium
3+: Ce
3+: Cr
3+: the YAG crystal is packed in crucible, uses the alumina powder landfill, does not allow Nd
3+: Ce
3+: Cr
3+: the YAG crystal exposes, and insulation, keep a public place clean;
(2) close door of annealing furnace, vacuumize, be filled with high-purity argon gas protection in annealing furnace;
(3) at first with the speed of 100 ℃/hour, be warming up to 400 ℃, then with the speed of 50-70 ℃/hour, be warming up to 1250 ℃, constant temperature 36 hours;
(4) with the speed of 5-20 ℃/hour, be cooled to 1000 ℃, then per hour than the cooling rate of falling 15 ℃ last hour, to be cooled to 150-200 ℃ more;
(5) powered-down, take out Nd while naturally being cooled to 30 ℃ in stove
3+: Ce
3+: Cr
3+: the YAG crystal.
The crystal taken out is detected with 20 milliwatt green glows, and the scattering particles of crystal are eliminated fully.Then with the cross-polarized light stressometer, detect crystal stress basically eliminate.In addition, the crystal appearance color does not change, and shows Cr
3+Ion does not change into Cr
4+Ion.
Embodiment five
The method for annealing of the yag crystal of the disclosed a kind of neodymium-doped of the present embodiment, cerium and chromium, comprise the steps:
(1) get carbon fiber crucible, put into the annealing furnace Frequency Induction Heating, then by the yttrium aluminum garnet Nd of neodymium-doped, cerium and chromium
3+: Ce
3+: Cr
3+: the YAG crystal is packed in crucible, uses the alumina powder landfill, does not allow Nd
3+: Ce
3+: Cr
3+: the YAG crystal exposes, and insulation, keep a public place clean;
(2) close door of annealing furnace, vacuumize, be filled with high-purity argon gas protection in annealing furnace;
(3) at first with the speed of 100 ℃/hour, be warming up to 400 ℃, then with the speed of 50-70 ℃/hour, be warming up to 1200 ℃, constant temperature 12 hours;
(4) with the speed of 5-20 ℃/hour, be cooled to 1000 ℃, then per hour than the cooling rate of falling 10 ℃ last hour, to be cooled to 150-200 ℃ more;
(5) powered-down, take out Nd while naturally being cooled to 30 ℃ in stove
3+: Ce
3+: Cr
3+: the YAG crystal.
The crystal taken out is detected with 20 milliwatt green glows, and the scattering particles of crystal eliminate 70%.Then with the cross-polarized light stressometer, detect crystal stress basically eliminate.In addition, the crystal appearance color does not change, and shows Cr
3+Ion does not change into Cr
4+Ion.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (2)
1. the method for annealing of the yag crystal of a neodymium-doped, cerium and chromium, is characterized in that, comprises the steps:
(1) get carbon fiber crucible, put into the annealing furnace Frequency Induction Heating, then by the yttrium aluminum garnet Nd of neodymium-doped, cerium and chromium
3+: Ce
3+: Cr
3+: the YAG crystal is packed in crucible, uses the alumina powder landfill, does not allow Nd
3+: Ce
3+: Cr
3+: the YAG crystal exposes, and insulation, keep a public place clean;
(2) close door of annealing furnace, vacuumize, be filled with high-purity argon gas protection in annealing furnace;
(3) at first with the speed of 100 ℃/hour, be warming up to 400 ℃, then with the speed of 50-70 ℃/hour, be warming up to 1200-1300 ℃, constant temperature 12 hours-36 hours;
(4) with the speed of 5-20 ℃/hour, be cooled to 1000 ℃, then per hour than the cooling rate of falling 10-15 ℃ last hour, to be cooled to 150-200 ℃ more;
(5) powered-down, take out Nd while naturally being cooled to 30 ℃ in stove
3+: Ce
3+: Cr
3+: the YAG crystal.
2. the method for annealing of the yag crystal of a kind of neodymium-doped as claimed in claim 1, cerium and chromium, is characterized in that, in described step (3), is constant temperature 24 hours at 1250 ℃ of temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198400A (en) * | 2015-10-12 | 2015-12-30 | 长春理工大学 | Medium-frequency induction sintering method for neodymium-doped yttrium aluminum garnet laser ceramic |
| CN110117159A (en) * | 2019-06-27 | 2019-08-13 | 浦江县恒凯水晶有限公司 | A kind of artificial lotus crystalline substance and preparation method thereof |
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| CN101944703A (en) * | 2010-07-30 | 2011-01-12 | 北京工业大学 | Preparation process of laser rod terminated with Cr4+:YAG |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198400A (en) * | 2015-10-12 | 2015-12-30 | 长春理工大学 | Medium-frequency induction sintering method for neodymium-doped yttrium aluminum garnet laser ceramic |
| CN110117159A (en) * | 2019-06-27 | 2019-08-13 | 浦江县恒凯水晶有限公司 | A kind of artificial lotus crystalline substance and preparation method thereof |
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