CN101319392B - Hafnium iron manganese three-doped lithium niobate crystal and method of producing the same - Google Patents
Hafnium iron manganese three-doped lithium niobate crystal and method of producing the same Download PDFInfo
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- CN101319392B CN101319392B CN2008100549526A CN200810054952A CN101319392B CN 101319392 B CN101319392 B CN 101319392B CN 2008100549526 A CN2008100549526 A CN 2008100549526A CN 200810054952 A CN200810054952 A CN 200810054952A CN 101319392 B CN101319392 B CN 101319392B
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- lithium niobate
- hafnium
- niobate crystal
- doped lithium
- iron manganese
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Abstract
The invention provides a lithium niobate crystal doped with hafnium, iron and manganese and a preparation method thereof. The composition of the lithium niobate crystal doped with the hafnium iron and manganese is LiaNbbO3:Fec:Mnd:Hfe, wherein, a is between 0.934360 and 0.945525, b is 1.00000, c is between 0.00156250 and 0.003125, d is between 0.000234700 and 0.0004694, e is between 0.0450000 and0.0600000, and the idiogenous mixture ratio of [Li]/[Nb] is between 0.934360 and 0.945525. The preparation method comprises the following steps that: Li2CO3, Nb2O5, Fe2O3, MnO and HfO2 are mixed evenly according to a ratio of 9.38000:10.000:0.0078125:0.002347:0.04000 and dried, and the mixture is calcined at a temperature of 1100 DEG C for 2 hours so that a polycrystal powder material is prepared; the polycrystal powder material is heated and melted, the lithium niobate crystal doped with the hafnium, iron, manganese is grown by the Czochralski method through pulling, shouldering, being isometric and ending along a C axis direction, the puling speed is between 1 and 3 millimeters per hour, the rotating speed is between 15 and 30rpm, the gas-liquid difference in temperature is 20 DEG C, the temperature gradient in the fused mass is 1.5 DEG C per millimeter, and the difference in temperature on the upper part of the fused mass is 1 DEG C per millimeter; and the grown crystal is subjected to poling, annealing, polishing and cutting at a temperature of 1200 DEG C so that the lithium niobate crystal doped with the hafnium, iron and manganese used for storing is prepared. The method solves the problems that a three-dimensional holographic memory has long response time and information volatility, increases the response speed, and simultaneously ensures that the information is not wiped off in the information reading process, thereby having great market prospect.
Description
Technical field
The present invention relates to the lithium niobate crystals in a kind of photoelectric crystal field and preparation method thereof, specifically, is that the Lithium niobium trioxide three that a kind of photoelectric crystal light is sold off is mixed crystal and preparation method thereof.
Background technology
Three-dimensional holographic storage substitutes present storer at last, becomes the information recording medium of a new generation.But the greatest problem that this product faces at present is to can not find suitable storage medium.
In the CN1277271 patent, Li has been proposed
1-xNb
1+yO
3: Fe
m: M
nTwo crystal of mixing, wherein M is a kind of of Mg, Zn, In anti-photorefraction doped element.Along with the mixing of M impurity, can improve the monochromatic Hologram Storage performance of crystalline in this patent, for example, improve anti-light scattering ability, reduce the scattering of light threshold value, shorten the time of response.But these crystalline light are sold off the more single doped iron lithium niobate crystal of diffraction efficiency and are significantly decreased.
People such as Kokanyan are at " Reduced photorefraction in hafnium-doped single-domain and periodicallypoled lithium niobate crystals ", Appl.Phys.Lett.84,1880 (2004), found a kind of new tetravalence anti-photorefraction doped element, when mixing HfO
2Amount when reaching threshold concentration 4mol%, its anti-photorefraction ability can match in excellence or beauty with highly magnesium-doped lithium niobate crystals.Japanese plum very waits the people at " Enhanced photorefractive properties of LiNbO
3: Fe crystals by HfO
2Co-doping ", Appl.Phys.Lett., 89 (10), 101126 (2006), reported LiNbO
3: the two crystalline photorefractive properties of mixing of Fe:Hf have also obtained significantly improving, both kept fast response speed, guaranteed very high diffraction efficiency again, the incorporation of wherein going back ortho states be 5mol%Hf two to mix the crystalline time of response be 2.6s, diffraction efficiency is 45.4%.This shows that the Hf ionic mixes and will obviously improve the photorefractive property of doped iron lithium niobate crystal.But, LiNbO
3: mix the volatility problem that crystal can not solve information in reading process for Fe:Hf pair.
Nineteen nineties, K.Buse, A.Abidi, D.Psaltisza have invented and have a kind ofly utilized that ferrimanganic is two to be mixed or the photochromy sex change of copper cerium double-doped lithium niobate crystal realizes non-volatile full optical storage method (the U.S Patent No.6 that reads of information, 157,470).People such as K.Buse are at Nature, and 393,665 (1998), reported LiNbO in " Non-Volatile Holographic storage in doubly dopedlithium niobate crystals "
3: the double-colored non-volatile Hologram Storage of Fe:Mn, solved the volatility problem of information, but also introduced the slow deficiency of response speed simultaneously, the saturation response time is about 60 minutes, and this will be difficult to satisfy people's requirement to access speed when the real time access of the information of carrying out.
Improvement is sold off the Hologram Storage performance with the light of optimizing lithium niobate crystals, will solve simultaneously especially that response speed is slow, the volatile problem of information is the problem that people thirst for solving.
Summary of the invention
The purpose of this invention is to provide a kind of hafnium iron manganese three-doped lithium niobate crystal and preparation method thereof, solving the volatility problem of oversize and information of three-dimensional holographic storage time of response in the access procedure of information, thereby make it can really be used for the real time access of information and information can also be preserved when being read repeatedly for a long time.
Hafnium iron manganese three-doped lithium niobate crystal of the present invention, its composition is expressed as Li
aNb
bO
3: Fe
c: Mn
d: Hf
e
Wherein, a=0.934360～0.945525, b=1.00000, c=0.00156250～0.003125, d=0.000234700～0.0004694, e=0.0400000～0.0600000;
Congruent proportioning [Li]/[Nb]=0.934360～0.945525.
The preparation method of hafnium iron manganese three-doped lithium niobate crystal of the present invention, this method follow these steps to carry out:
(1) by the metering ratio of above-mentioned each element, takes by weighing Li
2CO
3, Nb
2O
5, Fe
2O
3, MnO and HfO
2, to dry and mix, back 1100 ℃ of calcinings obtain the polycrystalline powder;
(2) the hafnium iron manganese three-doped lithium niobate polycrystalline powder fusing that step (1) is obtained, with Czochralski method growth hafnium ferrimanganic lithium niobate crystals, its pulling rate is 1～3mm/h, rotating speed is 15～30rpm, thermograde is 1.5 ℃/mm in 20 ℃ of the gas-liquid temperature differences, melt, and the melt top temperature difference is 1 ℃/mm;
(3) hafnium iron manganese three-doped lithium niobate crystal that step (2) is obtained carries out poling, annealing at 1200 ℃, after polish, cut, obtain the hafnium iron manganese three-doped lithium niobate crystal that is used to store;
The preparation method of hafnium iron manganese three-doped lithium niobate crystal of the present invention, this method mix iron, manganese, hafnium metal ion simultaneously in lithium niobate crystals, its concrete grammar is to follow these steps to carry out:
(1) by the metering ratio of above-mentioned each element, takes by weighing purity and be 99.99% Li
2CO
3, Nb
2O
5, Fe
2O
3, MnO, HfO
2, at 2 hours following drying materials of 150 ℃ of constant temperature, mix then, 800 ℃ of constant temperature two hours, make Li
2CO
3Decompose,, obtain the polycrystalline powder of hafnium iron manganese three-doped lithium niobate crystal 1100 ℃ of calcinings 2 hours;
(2) platinum crucible is put in the hafnium iron manganese three-doped lithium niobate polycrystalline powder compacting that step (1) is obtained, and all melts up to powder with Frequency Induction Heating; With the Czochralski method along the C direction of principal axis according to drawing process growth hafnium iron manganese three-doped lithium niobate crystals such as neck, shouldering, isometrical, ending; Pulling rate is 1～3mm/h in the process of lifting, and rotating speed is 15～30rpm, and thermograde is 1.5 ℃/mm in 20 ℃ of the gas-liquid temperature differences, melt, and the melt top temperature difference is 1 ℃/mm;
(3) hafnium iron manganese three-doped lithium niobate crystal that step (2) is obtained carries out poling, annealing under 1200 ℃, polishes at last, cuts, and obtains the hafnium iron manganese three-doped lithium niobate crystal that is used to store.
Hafnium iron manganese three-doped lithium niobate crystal provided by the invention obtained significantly improving because the Hf ionic mixes shallow center Fe ionic photorefractive property, and the photorefractive property at shallow center directly determines the response speed of double-colored non-volatile Hologram Storage.Therefore, the hafnium iron manganese three-doped lithium niobate crystal time of response volatility problem long and information in reading process that can solve present three-dimensional holographic storage simultaneously and run into.
The hafnium iron manganese three-doped lithium niobate crystal that obtains according to the method described above can be used in double-colored non-volatile Hologram Storage.Have huge market outlook.
Embodiment
Below in conjunction with specific embodiment the specific embodiment of the present invention is further detailed
Embodiment 1
(1) takes by weighing purity and be Li
2CO
3, Nb
2O
5, Fe
2O
3, MnO, HfO
2, by 9.34360: 10.000: 0.0078125: 0.004694: 0.5000, at 2 hours following drying materials of 200 ℃ of constant temperature, thorough mixing 24 hours on mixer then 800 ℃ of constant temperature two hours, made Li
2CO
3Fully decompose,, obtain the polycrystalline powder of hafnium iron manganese three-doped lithium niobate crystal 1100 ℃ of calcinings 2 hours.
(2) platinum crucible is put in the hafnium iron manganese three-doped lithium niobate polycrystalline powder compacting that step (1) is obtained, and utilizes Frequency Induction Heating all to melt up to powder.Use the Czochralski method along the C direction of principal axis according to drawing process growth hafnium iron manganese three-doped lithium niobate crystals such as neck, shouldering, isometrical, ending.Pulling rate is 1～3mm/h in the process of lifting, and rotating speed is 15～30rpm, and thermograde is 1.5 ℃/mm in 20 ℃ of the gas-liquid temperature differences, melt, and the melt top temperature difference is 1 ℃/mm.
(3) hafnium iron manganese three-doped lithium niobate crystal that step (2) is obtained carries out poling, annealing under 1200 ℃.Polish at last, cut, obtain the hafnium iron manganese three-doped lithium niobate crystal that is used to store, its composition is expressed as Li
aNb
bO
3: Fe
c: Mn
d: Hf
e, a=0.934360 wherein, b=1.00000, c=0.00078125, d=0.0004694, e=0.0500000, congruent proportioning [Li]/[Nb]=0.934360.
Embodiment 2
The preparation method of hafnium iron manganese three-doped lithium niobate crystal is to mix metal ions such as iron, manganese, hafnium in lithium niobate crystals simultaneously, and its concrete grammar follows these steps to carry out:
(1) takes by weighing purity and be 99.99% Li
2CO
3, Nb
2O
5, Fe
2O
3, MnO, HfO
2, by 9.38000: 10.000: 0.015625: 0.00234: 0.4500, at 2 hours following drying materials of 150 ℃ of constant temperature, thorough mixing 24 hours on mixer then 800 ℃ of constant temperature two hours, made Li
2CO
3Fully decompose,, obtain the polycrystalline powder of hafnium iron manganese three-doped lithium niobate crystal 1100 ℃ of calcinings 2 hours.
(2) platinum crucible is put in the hafnium iron manganese three-doped lithium niobate polycrystalline powder compacting that step (1) is obtained, and utilizes Frequency Induction Heating all to melt up to powder.Use the Czochralski method along the C direction of principal axis according to drawing process growth hafnium iron manganese three-doped lithium niobate crystals such as neck, shouldering, isometrical, ending.Pulling rate is 1～3mm/h in the process of lifting, and rotating speed is 15～30rpm, and thermograde is 1.5 ℃/mm in 20 ℃ of the gas-liquid temperature differences, melt, and the melt top temperature difference is 1 ℃/mm.
(3) hafnium iron manganese three-doped lithium niobate crystal that step (2) is obtained carries out poling, annealing under 1200 ℃.Polish at last, cut, obtain the hafnium iron manganese three-doped lithium niobate crystal that is used to store, its composition is expressed as Li
aNb
bO
3: Fe
c: Mn
d: Hf
e, a=0.938000 wherein, b=1.00000, c=0.00156250, d=0.000234700, e=0.0450000, congruent proportioning [Li]/[Nb]=0.938000.
Embodiment 3
(1) takes by weighing Li
2CO
3, Nb
2O
5, Fe
2O
3, MnO, HfO
2, by 9.40000: 10.000: 0.00850000: 0.003694: 0.6000, at 2 hours following drying materials of 200 ℃ of constant temperature, thorough mixing 24 hours on mixer then 900 ℃ of constant temperature two hours, made Li
2CO
3Fully decompose,, obtain the polycrystalline powder of hafnium iron manganese three-doped lithium niobate crystal 1100 ℃ of calcinings 2 hours.
(2) platinum crucible is put in the hafnium iron manganese three-doped lithium niobate polycrystalline powder compacting that step (1) is obtained, and utilizes Frequency Induction Heating all to melt up to powder.With the Czochralski method along the C direction of principal axis according to drawing process growth three-doped lithium niobate crystals such as neck, shouldering, isometrical, ending.Pulling rate is 1～3mm/h in the process of lifting, and rotating speed is 15～30rpm, and thermograde is 1.5 ℃/mm in 20 ℃ of the gas-liquid temperature differences, melt, and the melt top temperature difference is 1 ℃/mm.
(3) hafnium iron manganese three-doped lithium niobate crystal that step (2) is obtained carries out poling, annealing under 1200 ℃.Polish at last, cut, obtain the hafnium iron manganese three-doped lithium niobate crystal that is used to store, its composition is expressed as Li
aNb
bO
3: Fe
c: Mn
d: Hf
e, a=0.940000 wherein, b=1.00000, c=0.000850000, d=0.0003694, e=0.0600000, congruent proportioning [Li]/[Nb]=0940000.
Claims (3)
1. hafnium iron manganese three-doped lithium niobate crystal, its composition is expressed as Li
aN
bBO
3: Fe
c: Mn
d: Hf
e
Wherein, a=0.934360～0.945525, b=1.00000, c=0.00156250～0.003125, d=0.000234700～0.0004694, e=0.0400000～0.0600000;
Congruent proportioning [Li]/[Nb]=0.934360～0.945525.
2. preparation method who is used for the described hafnium iron manganese three-doped lithium niobate crystal of claim 1 is characterized in that this method is to follow these steps to carry out:
(1) by the metering ratio of described each element of claim 1, takes by weighing Li
2CO
3, Nb
2O
5, Fe
2O
3, MnO and HfO
2, to dry and mix, back 1100 ℃ of calcinings obtain hafnium iron manganese three-doped lithium niobate crystal polycrystalline powder;
(2) the hafnium iron manganese three-doped lithium niobate crystal polycrystalline powder fusing that step (1) is obtained, with Czochralski method growth hafnium iron manganese three-doped lithium niobate crystal, its pulling rate is 1～3mm/h, rotating speed is 15～30rpm, 20 ℃ of gas-liquid temperature differences, thermograde is 1.5 ℃/mm in the melt, and the melt top temperature difference is 1 ℃/mm;
(3) hafnium iron manganese three-doped lithium niobate crystal that step (2) is obtained carries out poling, annealing at 1200 ℃, after polish, cut, obtain the hafnium iron manganese three-doped lithium niobate crystal that is used to store.
3. the preparation method of hafnium iron manganese three-doped lithium niobate crystal as claimed in claim 2 is characterized in that mixing simultaneously in this lithium niobate crystals iron, manganese, hafnium metal ion, and its concrete grammar follows these steps to carry out:
(1) by the metering ratio of described each element of claim 1, takes by weighing purity and be 99.99% Li
2CO
3, Nb
2O
5, Fe
2O
3, MnO, HfO
2, at 2 hours following drying materials of 150 ℃ of constant temperature, mix then, 800 ℃ of constant temperature two hours, make Li
2CO
3Decompose fully,, obtain the polycrystalline powder of hafnium iron manganese three-doped lithium niobate crystal 1100 ℃ of calcinings 2 hours;
(2) platinum crucible is put in the hafnium iron manganese three-doped lithium niobate polycrystalline powder compacting that step (1) is obtained, and all melts up to powder with Frequency Induction Heating; With the Czochralski method along the C direction of principal axis according to drawing neck, shouldering, isometrical, epilog growth hafnium iron manganese three-doped lithium niobate crystal; Pulling rate is 1～3mm/h in the process of lifting, and rotating speed is 15～30rpm, and thermograde is 1.5 ℃/mm in 20 ℃ of the gas-liquid temperature differences, melt, and the melt top temperature difference is 1 ℃/mm;
(3) hafnium iron manganese three-doped lithium niobate crystal that step (2) is obtained carries out poling, annealing under 1200 ℃, after polish, cut, obtain being used for the hafnium iron manganese three-doped lithium niobate crystal of 3D hologram storage.
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Non-Patent Citations (2)
| Title |
|---|
| Luca Razzari1等.Reduced photorefraction in Hafnium-doped single-domain and periodically-poled lithium niobate crystals.《Conference on Lasers and Electro-Optics (CLEO)》.2004,第2卷 * |
| 徐晓麟.镁锰铁掺杂铌酸锂晶体的生长和结构分析.《中国优秀博硕士学位论文全文数据库 (硕士)工程科技Ⅰ辑 》.中国知网,2007,(第1期),B020-42. * |
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Inventor after: Li Xiaochun Inventor after: Cui Caie Inventor after: Yi Xuezhuan Inventor after: Xia Xiongying Inventor after: Wang Zhe Inventor after: Zhou Jinwen Inventor after: Shi Feng Inventor after: Wang Longsheng Inventor before: Li Xiaochun Inventor before: Yi Xuezhuan Inventor before: Xia Xiongying Inventor before: Wang Zhe Inventor before: Zhou Jinwen Inventor before: Shi Feng Inventor before: Wang Longsheng |
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