CN100467678C - Hf:Er:LiNbO3 crystal and preparation method thereof - Google Patents

Hf:Er:LiNbO3 crystal and preparation method thereof Download PDF

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CN100467678C
CN100467678C CNB2007100716990A CN200710071699A CN100467678C CN 100467678 C CN100467678 C CN 100467678C CN B2007100716990 A CNB2007100716990 A CN B2007100716990A CN 200710071699 A CN200710071699 A CN 200710071699A CN 100467678 C CN100467678 C CN 100467678C
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crystal
hfo
linbo
lico
doping
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CN101037801A (en
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孙亮
徐玉恒
国凤云
吕强
于海涛
李洪涛
蔡伟
赵连城
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Yibin University
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Harbin Institute of Technology
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Abstract

A Hf:Er:LiNbO3 crystal and its preparing method, belongs to a crystal ant its preparing method. The invention solves the problem that magnesium and zinc are intermingled to improve the anti-light-damage capacity of lithium niobate crystal, with a premise that itself good capability of lithium niobate crystal is kept, but itself good optical capability of the crystal is suppressed. The inventive Hf:Er:LiNbO3 crystal is made of HfO2, Er2O3, Nb2O5 and LiCO3, which are all the purity of 99.99%; in which the intermingled amount of HfO2 is 2-6 mol% by the total amount of HfO2, Er2O3, Nb2O5 and LiCO3, the intermingled amount of Er2O3 is 0.5-2 mol % by the total amount of HfO2, Er2O3, Nb2O5 and LiCO3, and the mol ratio of Li and Nb is 0.964. The preparing method includes: (1) weighing and mixing HfO2, Er2O3, Nb2O5 and LiCO3; (2) growing the crystal by the pulling method; (3) polarizing; (4) polishing the crystal under surface optical quality class after cutting it to produce a Hf:Er:LiNbO3 crystal. The inventive Hf:Er:LiNbO3 crystal has high glossiness and is uniform, with no flaw, growing strip and crack. The inventive method for producing the Hf:Er:LiNbO3 crystal is simple and is easy to operate, and has rapid growing speed of the crystal.

Description

Hf:Er:LiNbO 3Crystal and preparation method thereof
Technical field
The present invention relates to a kind of crystal and preparation method thereof.
Background technology
Converted light source is widely used in HIGH-DENSITY OPTICAL STORAGE, coloured plate demonstration, photoelectronics and medical diagnosis on the solid-state green glow.Up to now, in many crystalline materials, had been found that green glow up-conversion luminescence phenomenon.And Er:LiNbO 3Crystal is exactly this wherein important, and this is because the trivalent erbium ion as a kind of active ions in the up-conversion luminescent material, has high up-conversion luminescence efficient; Lithium niobate crystals has good piezoelectricity, ferroelectric, photoelectricity, non-linear and photorefractive property, therefore, and Er:LiNbO 3Crystal is the rare crystalline material that integrates the premium properties of er element and lithium niobate crystals.Because Er:LiNbO 3Crystalline is used with scientific research and is worth, and many investigators turn to this traditional crystalline material of Lithium niobium trioxide to sight again.In the up-conversion luminescence process, the radiationless transition probability of some intermediate levels is more little, and fluorescence lifetime is just long more, and is just favourable more to up-conversion luminescence.Therefore, how improving the fluorescence lifetime of changing on the green glow, is the important directions of improving conversion solid statelaser performance on the green glow.Past is for Er:LiNbO 3The crystal raising of performance in this respect more is confined to the improvement of the device preparation technology in later stage, and in fact, the optimization in Properties of device base mateiral more should be the focus that we improve for transfer capability on the green glow.Although, Er:LiNbO 3Crystal has above-mentioned many advantages, still, because the photo-damage resistance of lithium niobate crystals itself is lower, seriously limit its application in actual production, usually, adopt doping photodamage resistant element magnesium, zinc etc., improve perhaps that niobium lithium ratio overcomes this shortcoming in the lithium niobate crystals.But, traditional photodamage resistant doping agent must be under high density, for example, the concentration of magnesium is 5mol% (photodamage resistant thresholding concentration), and the higher 6.5mol% of the requirement of zinc, competence exertion photodamage resistant effect, in the real crystal growth, mixing of the photodamage resistant doping agent of high density makes crystal be difficult to growth, for example, component fractional condensation that the crystal composition heterogeneity of growth, the appearance of striation, crystal break easily, occur in the polarization process etc. has a strong impact on the phenomenon of crystal mass; Simultaneously, the doping of high density has been suppressed the good performance that lithium niobate crystals itself has, for example, at the Hologram Storage aspect of performance, the photodamage resistant doping agent of high density, although make lithium niobate crystals obtain good photodamage resistant performance, serious reduction diffraction efficiency, this be realize the storage of magnanimity optical information do not wish to see; Again for example, the magnesium doping Er:LiNbO of high density 3Crystalline fluorescence lifetime sharply reduces, and this is Er:LiNbO 3Crystal least is ready to see on solid statelaser is used.In fact, the past, adulterated research more was confined to how to improve the raising of the photo-damage resistance of crystal itself for photodamage resistant, and had ignored the photodamage resistant doping agent for LiNbO 3The influence of the optical property of crystal others.Therefore, need find a kind of photodamage resistant element to have low photodamage resistant thresholding concentration, more need the lithium niobate crystals performance being expanded to the performance of paying close attention to others for photodamage resistant element.
Summary of the invention
Though the objective of the invention is to have suppressed crystal itself and had good optical property in order to solve the photo-damage resistance that under the prerequisite that keeps the premium properties of lithium niobate crystals own magnesium-doped or zinc element has improved lithium niobate crystals; Near the lithium niobate crystals of stoichiometric ratio be difficult to grow and the Crystal Growth of Lithium Niobate speed of doping hafnium element slow, and crystal mass is poor, easy to crack, and a kind of Hf:Er:LiNbO that provides 3Crystal and preparation method thereof.Hf:Er:LiNbO of the present invention 3Crystal all is 99.99% HfO by purity 2, Er 2O 3, Nb 2O 5And LiCO 3Make; HfO wherein 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 32～6mol% of total amount of substance, Er 2O 3Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 30.5～2mol% of total amount of substance, the mol ratio of Li and Nb is 0.946.
The present invention prepares Hf:Er:LiNbO 3The step of crystal method is as follows: one, taking by weighing and mixing purity all is 99.99% HfO 2, Er 2O 3, Nb 2O 5And LiCO 3, HfO 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 32～6mol% of total amount of substance, Er 2O 3Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 30.5～2mol% of total amount of substance, the mol ratio of Li and Nb is 0.946; Two, adopt crystal pulling method to carry out crystal growth: the control pull rate is 0.8～1.5mm/h, and axial-temperature gradient is 40～50 ℃/cm, and speed of rotation is 15～25r/min; Three, polarization: it is 1160～1200 ℃ that the crystal that grows is placed temperature, and current density is 5mA/cm 2Condition under the 30 ± 2min that polarizes; Four, accurately directed the crystal after the polarization, and according to Y face sliced crystal cutting back the optical quality level is carried out on its surface and polish, Hf:Er:LiNbO promptly obtained 3Crystal.
Hf:LiNbO 3The performance of the photodamage resistant that crystal is good, photodamage resistant thresholding concentration only are 4mol%.The Hf element effectively raises the photodamage resistant performance of lithium niobate crystals, simultaneously, and the premium properties that compacting lithium niobate crystals within reason again itself has.Measure Hf:Er:LiNbO of the present invention 3Crystalline up-conversion fluorescence performance, result are presented at emission spectrum peak, 500～600nm place band strength than Er:LiNbO 3Crystal has improved 56.1% at least, and multipotency mentions 188%, Hf:Er:LiNbO 3Crystal in the fluorescence lifetime at 550nm place than Er:LiNbO 3The crystal phenomenal growth, the longest growth has reached 39.2%, and the 5mol%Mg:1mol%Er:LiNbO that has reported 3Crystal in the fluorescence lifetime at 550nm place than Er:LiNbO 3The shortening of crystal rapid deterioration has reduced 82.2%.As seen, Hf:Er:LiNbO 3Crystal not only has strong photo-damage resistance, and fluorescence property not only do not worsen by the photodamage resistant doping agent, significantly improves Hf:Er:LiNbO on the contrary 3Crystal is applied to the good base mateiral of conversion solid statelaser on the green glow.
Hf:Er:LiNbO of the present invention 3The crystalline preparation method is simple, is convenient to operation, and crystalline growth velocity is fast.
Description of drawings
Fig. 1 is a crystallogram of the present invention; Fig. 2 is 1mol%Er:LiNbO 3The spectrogram of crystal up-conversion fluorescence; Fig. 3 is 2mol%Hf:1mol%Er:LiNbO 3The spectrogram of crystal up-conversion fluorescence; Fig. 4 is 4mol%Hf:1mol%Er:LiNbO 3The spectrogram of crystal up-conversion fluorescence; Fig. 5 is 6mol%Hf:1mol%Er:LiNbO 3The spectrogram of crystal up-conversion fluorescence; Fig. 6 is 1mol%Er:LiNbO 3Crystal is at the figure as a result of 550nm place fluorescence power extinction curve and the match of single e index fluorescence lifetime, among the figure-and ■-expression 1mol%Er:LiNbO 3Crystal is at 550nm place fluorescence power extinction curve, among the figure-and the matched curve of the single e index fluorescence lifetime of expression; Fig. 7 is 2mol%Hff:1mol%Er:LiNbO 3Crystal is at the figure as a result of 550nm place fluorescence power extinction curve and the match of single e index fluorescence lifetime, among the figure-and ■-expression 2mol%Hf:1mol%Er:LiNbO 3Crystal is at 550nm place fluorescence power extinction curve, among the figure-and the matched curve of the single e index fluorescence lifetime of expression; Fig. 8 is 4mol%Hf:1mol%Er:LiNbO 3Crystal is at the figure as a result of 550nm place fluorescence power extinction curve and the match of single e index fluorescence lifetime, among the figure-and ■-expression 4mol%Hf:1mol%Er:LiNbO 3Crystal is at 550nm place fluorescence power extinction curve, among the figure-and the matched curve of the single e index fluorescence lifetime of expression; Fig. 9 is 6mol%Hf:1mol%Er:LiNbO 3Crystal is at the figure as a result of 550nm place fluorescence power extinction curve and the match of single e index fluorescence lifetime, among the figure-and ■-expression 6mol%Hf:1mol%Er:LiNbO 3Crystal is at 550nm place fluorescence power extinction curve, among the figure-and the matched curve of the single e index fluorescence lifetime of expression.
Embodiment
Embodiment one: present embodiment Hf:Er:LiNbO 3Crystal all is 99.99% HfO by purity 2, Er 2O 3, Nb 2O 5And LiCO 3Make; HfO wherein 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 32～6mol% of total amount of substance, Er 2O 3Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 30.5～2mol% of total amount of substance, the mol ratio of Li and Nb is 0.946.
Embodiment two: HfO in the present embodiment 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 3The 2mol% of total amount of substance.Present embodiment is identical with embodiment one.
Embodiment three: HfO in the present embodiment 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 3The 4mol% of total amount of substance.Present embodiment is identical with embodiment one.
Embodiment four: HfO in the present embodiment 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 3The 6mol% of total amount of substance.Present embodiment is identical with embodiment one.
Embodiment five: Er in the present embodiment 2O 3Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 3The 1mol% of total amount of substance.Present embodiment is identical with embodiment one.
Embodiment six: Er in the present embodiment 2O 3Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 3The 1.5mol% of total amount of substance.Present embodiment is identical with embodiment one.
Embodiment seven: present embodiment Hf:Er:LiNbO 3Crystal prepares according to the following steps: one, taking by weighing and mixing purity all is 99.99% HfO 2, Er 2O 3, Nb 2O 5And LiCO 3, HfO 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 32～6mol% of total amount of substance, Er 2O 3Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 30.5～2mol% of total amount of substance, the mol ratio of Li and Nb is 0.946; Two, adopt crystal pulling method to carry out crystal growth: the control pull rate is 0.8～1.5mm/h, and axial-temperature gradient is 40～50 ℃/cm, and speed of rotation is 15～25r/min; Three, polarization: it is 1160～1200 ℃ that the crystal that grows is placed temperature, and current density is 5mA/cm 2Condition under the 30 ± 2min that polarizes; Four, accurately directed the crystal after the polarization, and according to Y face sliced crystal, the polishing of optical quality level is carried out to its surface in the cutting back, promptly obtains Hf:Er:LiNbO 3Crystal.
The crystal that present embodiment grows is pale pink, diameter 30mm, and height 20mm, glossiness height, uniform component, indefectible, no striation and flawless produce.
Embodiment eight: present embodiment is HfO in step 1 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 3The 2mol% of total amount of substance.Present embodiment is identical with embodiment seven.
Embodiment nine: present embodiment is HfO in step 1 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 3The 4mol% of total amount of substance.Present embodiment is identical with embodiment seven.
Embodiment ten: present embodiment is HfO in step 1 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 3The 6mol% of total amount of substance.Present embodiment is identical with embodiment seven.
Embodiment 11: present embodiment is Er in step 1 2O 3Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 3The 1mol% of total amount of substance.Present embodiment is identical with embodiment seven.
Embodiment 12: present embodiment is controlled pull rate in step 2 be 1～1.3mm/h, and axial-temperature gradient is 42～48 ℃/cm, and speed of rotation is 17～23r/min.Present embodiment is identical with embodiment seven.
Embodiment 13: present embodiment is controlled pull rate in step 2 be 1.2mm/h, and axial-temperature gradient is 45 ℃/cm, and speed of rotation is 20r/min.Present embodiment is identical with embodiment seven.
Embodiment 14: present embodiment is controlled pull rate in step 2 be 8mm/h, and axial-temperature gradient is 50 ℃/cm, and speed of rotation is 25r/min.Present embodiment is identical with embodiment seven.
Embodiment 15: present embodiment places temperature with the crystal that grows in step 3 be 1160 ℃, and current density is 5mA/cm 2Condition under the 30min that polarizes.Present embodiment is identical with embodiment seven.
Embodiment 16: in the present embodiment in step 3 crystal be that 1200 ℃, current density are 5mA/cm in temperature 2Polarize under the condition; (Z * X * Y) cutting, the cutting back is carried out the optical quality level to its surface and is polished according to 10mm * 8mm * 1.5mm the accurate orientation of crystal in step 4.Other is identical with embodiment.
The Hf:Er:LiNbO that Fig. 1 obtains for present embodiment 3Crystal, it is carried out optic test: adopt Ti: sapphire femtosecond pulse laser (Spitfire, Spectra-Physics), emission wavelength is that 800nm is an excitation light source, output rating is that 100mW, burst length are 120 femtoseconds, with ICCD is data-switching and gathering device, the life-time dilatation effect that causes in order to reduce to absorb again, incident light concentrates on the edge of wafer, the collection of exporting light is simultaneously also being carried out with surveying the edge, output be that visible green light wavelength is in 500～600nm scope.The fluorescence property result of test is shown in Fig. 2～9.Its comparing result is as follows:
(1) 1mol%Er:LiNbO 3Crystal, at the 550nm place, its relative intensity of fluorescence is 44.42, its fluorescence lifetime is 18.31 μ m.
(2) 2mol%Hf:1mol%Er:LiNbO 3Crystal, at the 550nm place, its relative intensity of fluorescence is 69.35, than 1mol%Er:LiNbO 3Crystal growing 56.1%; Its fluorescence lifetime is 24.24 μ m, than 1mol%Er:LiNbO 3Crystal growing 32.4%.
(3) 4mol%Hf:1mol%Er:LiNbO 3Crystal, at the 550nm place, its relative intensity of fluorescence is 98.10, than 1mol%Er:LiNbO 3Crystal growing 121%; Its fluorescence lifetime is 25.10 μ m, than 1mol%Er:LiNbO 3Crystal growing 37.1%.
(4) 6mol%Hf:1mol%Er:LiNbO 3Crystal, at the 550nm place, its relative intensity of fluorescence is 127.90, than 1mol%Er:LiNbO 3Crystal growing 188%; Its fluorescence lifetime is 25.49 μ m, than 1mol%Er:LiNbO 3Crystal growing 39.2%.
By above result as seen, doping Hf has improved conversion performance on the fluorescence under the prerequisite that keeps the premium properties of lithium niobate crystals own in lithium niobate crystals.

Claims (9)

1, a kind of Hf:Er:LiNbO 3Crystal is characterized in that it all is 99.99% HfO by purity 2, Er 2O 3, Nb 2O 5And LiCO 3Make; HfO wherein 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 32～6mol% of total amount of substance, Er 2O 3Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 30.5～2mol% of total amount of substance, the mol ratio of Li and Nb is 0.946.
2, Hf:Er:LiNbO according to claim 1 3Crystal is characterized in that HfO 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 3The 2mol% of total amount of substance.
3, Hf:Er:LiNbO according to claim 1 3Crystal is characterized in that HfO 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 3The 4mol% of total amount of substance.
4, Hf:Er:LiNbO according to claim 1 3Crystal is characterized in that HfO 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 3The 6mol% of total amount of substance.
5, Hf:Er:LiNbO according to claim 1 3Crystal is characterized in that Er 2O 3Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 3The 1mol% of total amount of substance.
6, Hf:Er:LiNbO as claimed in claim 1 3The crystalline preparation method is characterized in that Hf:Er:LiNbO 3Crystal prepares according to the following steps: one, taking by weighing and mixing purity all is 99.99% HfO 2, Er 2O 3, Nb 2O 5And LiCO 3, HfO 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 32～6mol% of total amount of substance, Er 2O 3Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 30.5～2mol% of total amount of substance, the mol ratio of Li and Nb is 0.946; Two, adopt crystal pulling method to carry out crystal growth: the control pull rate is 0.8～1.5mm/h, and axial-temperature gradient is 40～50 ℃/cm, and speed of rotation is 15～25r/min; Three, polarization: it is 1160～1200 ℃ that the crystal that grows is placed temperature, and current density is 5mA/cm 2Condition under the 30 ± 2min that polarizes; Four, accurately directed the crystal after the polarization, and according to Y face sliced crystal cutting back the optical quality level is carried out on its surface and polish, Hf:Er:LiNbO promptly obtained 3Crystal.
7, Hf:Er:LiNbO according to claim 6 3The crystalline preparation method is characterized in that HfO in step 1 2Doping be HfO 2, Er 2O 3, Nb 2O 5And LiCO 3The 4mol% of total amount of substance.
8, Hf:Er:LiNbO according to claim 6 3The crystalline preparation method is characterized in that the control pull rate is 1～1.3mm/h in step 2, and axial-temperature gradient is 42～48 ℃/cm, and speed of rotation is 17～23r/min.
9, Hf:Er:LiNbO according to claim 6 3The crystalline preparation method is characterized in that the control pull rate is 1.2mm/h in step 2, and axial-temperature gradient is 45 ℃/cm, and speed of rotation is 20r/min.
CNB2007100716990A 2007-01-26 2007-01-26 Hf:Er:LiNbO3 crystal and preparation method thereof Expired - Fee Related CN100467678C (en)

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CN103265954B (en) * 2013-05-16 2015-01-14 同济大学 Potassium-sodium niobate based oxide up-conversion luminescent material and preparation method thereof
CN103668458A (en) * 2013-12-31 2014-03-26 哈尔滨理工大学 Hafnium, neodymium, ytterbium and thulium doped lithium niobate crystal and preparation method thereof
CN103696010A (en) * 2013-12-31 2014-04-02 哈尔滨理工大学 Hafnium-dysprosium codoped lithium niobate crystal and preparation method thereof
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