CN103882524A - Preparation and application of ion-doped electro-optic crystal material - Google Patents

Preparation and application of ion-doped electro-optic crystal material Download PDF

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CN103882524A
CN103882524A CN201210555832.0A CN201210555832A CN103882524A CN 103882524 A CN103882524 A CN 103882524A CN 201210555832 A CN201210555832 A CN 201210555832A CN 103882524 A CN103882524 A CN 103882524A
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不公告发明人
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Abstract

The invention relates to growth and a preparation characterization method of an ion-doped electro-optical function crystal material, wherein the crystal has a general formula of M:KTa(1-x)NbxO3 (M is Fe, Cu, Co or Ni, and x is more than equal to 0.33 and is less than or equal to 0.5), and has a perovskite type structure, the Curie point is between -15-90 DEG C, and the ion doping concentration weight percentage is 0-0.5%. According to the present invention, the preparation is characterized in that a crystal pulling method is adopted to grow the crystal, the doped ion metal oxide is added between the primary sintering and the secondary sintering during the powder material preparation process, the appropriate prepared material design and the growth process are optimized to obtain the series of the M:KTa(1-x)NbxO3 crystals doped with different ions, and a determination method is provided for the quadratic electro-optic effect of the crystal; and the comparison results show that the quadratic electro-optic coefficient of the ion-doped M:KTN crystal is generally higher than the quadratic electro-optic coefficient of the pure KTN crystal so as to indicate that the electro-optic effect of the KTN crystal can be improved with ion doping.

Description

A kind of preparation and application of ion doping type Electrooptic crystal material
Technical field
The present invention relates to utilize preparation method and the application thereof of the synthetic a kind of novel ion doping crystalline material of metal oxide, belong to electric light functional crystal material research field.
Background technology
Electrooptic effect is the medium phenomenon that specific refractory power changes under the effect of extra electric field, utilize the electrooptic effect of crystalline material can realize the modulation of phase place, intensity and the propagation direction of light, Electro-optical Modulation is due to advantages such as high-level efficiency, fast-response and on-mechanicals (noninertia), be generally used for making the devices such as laser modulator, scanning device and photoswitch, be widely used in the high-grade, precision and advanced scientific research fields such as lidar, laser ranging, biomedical micro-imaging.Current widely used Electro-optical Modulation crystal is generally some and has the single shaft crystalline substance of linear electro-optic effect, as KDP, LN etc., but because the electro-optic coefficient of these crystal is less, the size of modulator and driving voltage are difficult to take into account simultaneously, conventionally need very high voltage just can obtain practical deflection angle, the efficiency of photoswitch is also lower, cannot meet application request.
KTa 1-x nb xo 3(be called for short: KTN) crystal is the known crystal with maximum secondary electrooptic effect, and its secondary electro-optic coefficient can reach 10 -14m 2/ V 2magnitude, be LN crystal nearly a hundred times, therefore the optics based on KTN crystal quadratic electro-optical effect reduce driving voltage, reduce to have more advantage aspect device size, more can meet the needs of following electro-optical device miniaturization, integrated development.Although the electro-optical properties of KTN crystal excellence is known already, due to growth conditions harshness, be difficult to obtain can practical application large size, high quality single crystal, the application of this crystal is very limited always.In recent years, due to the improvement of crystal growth technology of preparing, obtain remarkable progress for the growth of KTN crystal both at home and abroad, high quality, large size KTN monocrystalline are successfully obtained at present, crystal mass and size have reached element manufacturing requirement, along with the continuous maturation of crystal growth and complete processing, KTN crystal electric light unit modulation device progressively turns to product development and application stage from laboratory study.
Due to the unlimited solid solution feature of KTN crystal, be difficult to obtain the monocrystalline of high uniformity, an outstanding problem of restriction KTN crystal current optic component application is the beam divergence causing due to the component fluctuation of crystal at present, the in the situation that particularly and beam diameter long at light path being larger, be difficult to obtain gratifying modulation effect.Some metal ion mixing of bibliographical information can significantly improve the anaclasis deteriorated property of KTN crystal, inspired by this, for the electro-optical properties of optimizing KTN crystal is further to reduce device size, reducing crystal composition fluctuates to device application and designs the disadvantageous effect of bringing, the present invention is directed to the KTN crystal that Curie temperature is positioned near room temperature and carried out the research of metal ion mixing, obtain comparatively satisfied result, improved the secondary electro-optic coefficient of crystal, and then reduced modulating voltage.Up to now, there is not yet the report that utilizes ion doping method to optimize KTN crystal secondary electro-optical properties.
Summary of the invention
The present invention adopts the KTN crystal of Czochralski grown ion doping, through suitable batching design and growth technique optimization, has obtained the M:KTa of different ions doping 1-x nb xo 3(M=Fe, Cu, Co, Ni; 0.33≤ x≤ 0.5) serial crystal, and provide a kind of measuring method for the quadratic electro-optical effect of crystal.
Technical solution of the present invention is as follows:
One, M:KTa 1-x nb xo 3crystal
There is formula M: KTa 1-xnb xo 3electro-optic crystal, there is perovskite structure, wherein M=Fe, Cu, Co, Ni, and M content is 0 ~ 0.5 wt %; In crystal composition Nb content be 0.33≤ x≤ 0. 5, Curie temperature is positioned at-15 ~ 90 ° Cbetween, be Emission in Cubic at the above crystal of Curie temperature, m3m point group; Curie temperature becomes Tetragonal below, 4mm point group.The present invention preferably provides Cu:KTa 0.63 nb 0.37o 3, Cu:KTa 0.61 nb 0.39o 3, and Fe:KTa 0.62 nb 0.38o 3crystal, wherein:
Cu:KTa 0.63 nb 0.37o 3, 9.7 ° of C of Curie temperature, 1170 ° of C of fusing point; Cu:KTa 0.61 nb 0.39o 3, 24.2 ° of C of Curie temperature, 1160 ° of C of fusing point; Fe:KTa 0.62 nb 0.38o 3, 15.8 ° of C of Curie temperature, 1170 ° of C of fusing point.
Two, M:KTa 1-x nb xo 3the growth of crystal and preparation method
M:KTa of the present invention 1-xnb xo 3the preparation method of crystal, with high-purity K 2cO 3, Nb 2o 5, Ta 2o 5for raw material, with high-purity CuO, CoO, NiO and Fe 2o 3for dopant ion, adopt Czochralski grown, growing apparatus is induction heating pull-type single crystal growing furnace, crystal growth step is as follows:
(1), according to required crystal composition, select batching according to KT-KN sosoloid phasor, by K 2cO 3: (Nb 2o 5+ Ta 2o 5) according to mol ratio (1.1 ~ 1.2): 1 weighs, mix and be compacted into piece, with 950 ~ 1050 ° of C sintering 24 hours, grind into powder again after taking-up, added dopant ion oxide compound CuO, CoO, NiO or Fe according to 0 ~ 0.5% ratio of total mass now 2o 3.Again compacting through double sintering, obtains M:KTN polycrystal.
(2) in single crystal pulling stove, carry out crystal growth.Heating member is platinum crucible, and growth atmosphere is air atmosphere.Bulk polycrystal material is placed in to crucible, after shove charge, being warming up to 1150 ~ 1250 ° of C melts raw material, after overheated two hours, be lowered to seed crystal, through the neck-shouldering of sowing-receive-wait the processes such as neck growth, obtain M:KTN crystal, according to crystal composition difference, crystal growth temperature is between 1110 ~ 1200 ° of C, and the pull rate while waiting neck process of growth is 0.25 ~ 0.5 milli m/h, and crystalline substance turns 4 ~ 10 revs/min.Growth cycle 5 ~ 10 days.
(3) crystal growing process finishes, and fast crystal is lifted to melt liquid level, constant temperature 1 ~ 2 hour.Be positioned at the M:KTN crystal of room temperature following (Tc≤25 ° C) for Curie temperature, can be down to room temperature according to the rate of temperature fall of 10 ~ 15 ° of C/h always; And for the M:KTN crystal of Tc>25 ° of C, in the time being cooled to vicinity of Curie temperatures, rate of temperature fall need be adjusted to 1 ~ 2 ° of C/h and slowly be down to room temperature, rear taking-up crystal.
The growth method of in the past reporting ion doping type KTN crystal has molten-salt growth method, top seed crystal lifting method, and the present invention adopts Czochralski grown ion doping KTN crystal first, can obtain large size, high quality M:KTN crystalline material within a short period of time.
The M:KTN crystal that the present invention obtains is according to doping ionic species demonstration different from concentration different colours, as Cu:KTN crystal is generally blue-greenish colour or blueness, Fe:KTN crystal is generally yellow or tawny, more macrocrystal color is darker for ionic concn, in the time that dopant ion concentration is greater than 0.5wt%, crystal light transmission extreme difference, impact is used.
The ion doping type M:KTa that the present invention obtains 1-xnb xo 3crystal is a cube column, appear crystal face for [100] face family, this design and processing that is crystal has brought convenience, according to KTN crystal characteristic and the requirement of electro-optic crystal element, we define crystal growth direction be z to, processed sample orientation X square piece, Z square piece, (xyt) θ cut type θ=15 °, 30 °, 45 °, (xzt) θ cut type (xyt) θ=15 °, 30 °, 45 °.
Three, the measuring method of M:KTN crystal secondary electro-optic coefficient
The secondary electro-optic coefficient of KTN crystal is to describe the core parameter of electro-optical properties, and the relative permittivity of electro-optic coefficient and crystal is closely related, meet relation "
Figure 417217DEST_PATH_IMAGE001
", wherein ε 0be the specific inductivity in vacuum, be worth for 8.86pF/m; ε rit is the relative permittivity of crystal; G is the constant relevant with crystalline structure, g for the KTN crystal of perovskite structure 11=0.136 m 4/ C 2, g 12=-0.038m 4/ C 2.The relative permittivity of crystal can obtain according to the electric capacity of rectangular parallelepiped wafer, experimental program is to plate electrode on the relative two sides of crystal, so just form a parallel plate capacitor, M:KTN crystal is exactly dielectric medium wherein, with the electric capacity of this parallel plate capacitor of bridge measurement, by electric capacity and crystalline size, according to
Figure 396675DEST_PATH_IMAGE002
(C is the electric capacity of M:KTN crystal, and d and A are respectively thickness and the electrode area of wafer) calculates specific inductivity.
In the present invention, the concrete measuring method of M:KTN crystal specific inductivity is: first crystal is tangentially processed into rectangular parallelepiped piece according to difference, six mirror polish; The size range of the rectangular electrode end face length of side is 1 ~ 50mm, crystal thickness 0.5 ~ 10mm: electrode fabrication can adopt ion sputtering, vacuum evaporation and smear a kind of of three kinds of modes of conductive resin or increase in ion sputtering and vacuum evaporation metallic film surface the method that is coated with conductive resin, preferably the latter; Sample electric capacity can adopt LCR electric bridge or volt ohm-milliammeter to measure, preferably the former; Sample temperature control adopts TEC semiconductor temperature module.
The KTN crystal that do not adulterate is the same, the specific inductivity of M:KTN crystal of the present invention is influenced by ambient temperature obviously, can obtain best electro-optical properties at crystal vicinity of Curie temperatures, the specific inductivity of the M:KTN crystal that the present invention obtains is all the optimum dielectric constant measured at Curie temperature annex, different with dopant ion concentration according to crystal composition, relative permittivity value nearly 35000, not comparing with component KTN crystal of dopant ion, the specific inductivity of crystal under ion doping condition, secondary electro-optic coefficient can increase nearly 30%.
embodiment
Specific embodiment is below further illustrating that the present invention is made.Crystal growth raw material is the high-purity N b that Dongfang Tantalum Industry Co., Ltd., Ningxia Hui autonomy Region produces 2o 5, Ta 2o 5; High-purity K of Tianjin new pure chemistry reagent Research Institute 2cO 3; Doping oxide is high-purity CuO, the Fe that Aladdin reagent (Shanghai) Co., Ltd. produces 2o 3.Crystal growing apparatus used is the SKJ-50 type induction heating single crystal pulling stove that Shenyang Ke Jing Materials Technology Ltd. produces.
Embodiment 1:Cu:KTa 0.65nb 0.35o 3(Cu doping 0.1wt%)
By high-purity K 2cO 3, Ta 2o 5, Nb 2o 5according to mol ratio K 2cO 3: Ta 2o 5: Nb 2o 5=1.2:0.33:0.67 weigh batching, puts into platinum crucible after mixing briquetting, and in retort furnace, with 1050 ° of C sintering 24 hours, following reaction: 1.2K occurred raw material 2cO 3+ (Ta 2o 5, Nb 2o 5)=2K (Ta, Nb) O 3+ 0.2K 2o+1.2CO 2↑, obtain approximately 850 grams of KTN polycrystals, by polycrystal again grind into powder, add 0.85 gram of CuO powder and mix, briquetting, repeats a sintering process, obtains Cu:KTN polycrystal.
Cu:KTN polycrystal is placed in to platinum crucible, under air atmosphere, carries out crystal growing process.Adopt heating in medium frequency mode, be warming up to 1180 visible raw materials while spending and all melt, continue to be warming up to 1200 degree left and right, constant temperature 2 hours, after be cooled to 1175 degree, be lowered to seed crystal, through receiving neck, shouldering, isodiametric growth process, obtain the block Cu:KTa of rectangular parallelepiped 0.65nb 0.35o 3: crystal.In crystal growing process, crystalline substance turns and remains on 5 revs/min, pull rate 0.3 ~ 0.5mm/h, and isodiametric growth process temperature is controlled between 1170 ~ 1180 ° of C.Crystal growth finishes defensive position flowing mode and proposes crystal, and crystal leaves liquid level 2mm, keeps 5 revs/min of rotations, is down to room temperature with 15 ° of C/h.As required by crystal according to X square piece, Z square piece, (xyt) θ cut type θ=15 °, 30 °, 45 °, (xzt) θ cut type (xyt) θ=15 °, 30 °, 45 °, be processed into respectively 2mm × 3mm × 5mm wafer, be used for measuring the specific inductivity of crystal, see embodiment 10.
Embodiment 2:Cu:KTa 0.63nb 0.37o 3(Cu doping 0.25wt%)
The present embodiment crystal growth preparation process is substantially the same manner as Example 1, and difference is that proportioning raw materials is adjusted into K 2cO 3: Ta 2o 5: Nb 2o 5=1.2:0.31:0.69, approximately 800 grams of polycrystal total masses, CuO doping is adjusted into 2 grams, and the synthetic sintering temperature of polycrystal is adjusted into 1025 ° of C, and the temperature of sowing in crystal growing process is adjusted into 1165 ° of C left and right, and isodiametric growth temperature is adjusted into 1160 ~ 1170 ° of C; Crystal processing mode is identical with embodiment 1.
Embodiment 3:Cu:KTa 0.61nb 0.39o 3(Cu doping 0.25wt%)
The present embodiment crystal growth preparation process is substantially the same manner as Example 1, and difference is that proportioning raw materials is adjusted into K 2cO 3: Ta 2o 5: Nb 2o 5=1.1:0.29:0.71, approximately 800 grams of polycrystal total masses, CuO doping is adjusted into 2 grams, and the synthetic sintering temperature of polycrystal is adjusted into 1000 ° of C, and the temperature of sowing in crystal growing process is adjusted into 1145 ° of C left and right, and isodiametric growth temperature is adjusted into 1150 ~ 1160 ° of C; Crystal processing mode is identical with embodiment 1.
Embodiment 4:Co:KTa 0.58nb 0.42o 3(Cu doping 0.4wt%)
The present embodiment crystal growth preparation process is substantially the same manner as Example 1, and difference is that proportioning raw materials is adjusted into K 2cO 3: Ta 2o 5: Nb 2o 5=1.1:0.26:0.74, CoO content is adjusted into 3.2 grams, and crystal sintering temperature is adjusted into 1000 ° of C, and the temperature of sowing in crystal growing process is adjusted into 1140 ° of C left and right, and isodiametric growth temperature is adjusted into 1145 ~ 1150 ° of C; The present embodiment crystal Curie temperature is 45 ° of C, and higher than room temperature, for preventing crystal cleavage and reducing the generation on phase transformation farmland, when crystal is cooled to vicinity of Curie temperatures, rate of temperature fall is adjusted into 1 ° of C/h and slowly passes through Curie temperature, and crystal processing mode is identical with embodiment 1
Embodiment 5:Cu:KTa 0.5nb 0.5o 3(Cu doping 0.45wt%)
The present embodiment crystal growth preparation process is substantially the same manner as Example 4, and difference is that proportioning raw materials is adjusted into K 2cO 3: Ta 2o 5: Nb 2o 5=1.1:0.21:0.79, CuO content is adjusted into 3.5 grams, and crystal sintering temperature is adjusted into 950 ° of C, and the temperature of sowing in crystal growing process is adjusted into 1120 ° of C left and right, and isodiametric growth temperature is adjusted into 1115 ~ 1125 ° of C; Crystal processing mode is identical with embodiment 1.
Embodiment 6:Ni:KTa 0.67nb 0.33o 3(Fe doping 0.5wt%)
The present embodiment crystal growth preparation process is substantially the same manner as Example 1, and difference is that proportioning raw materials is adjusted into K 2cO 3: Ta 2o 5: Nb 2o 5=1.2:0.35:0.65, dopant ion changes to Ni 2o 3, doping is 4 grams, and crystal sintering temperature is adjusted into 1100 ° of C, and the crystal temperature of sowing is adjusted into 1180 ° of C, and growth temperature is adjusted into 1175 ~ 1190 ° of C; Crystal processing mode is identical with embodiment 1.
Embodiment 7:Fe:KTa 0.66nb 0.34o 3(Fe doping 0.25wt%)
The present embodiment crystal growth preparation process is substantially the same manner as Example 6, and difference is that proportioning raw materials is adjusted into K 2cO 3: Ta 2o 5: Nb 2o 5=1.15:0.32:0.68, dopant ion oxide compound Fe 2o 3amount is adjusted into 2 grams, and crystal sintering temperature is adjusted into 1080 ° of C, and the crystal temperature of sowing is adjusted into 1170 ° of C, and growth temperature is adjusted into 1165 ~ 1175 ° of C; Crystal processing mode is identical with embodiment 6
Embodiment 8:Fe:KTa 0.63nb 0.37o 3(Fe doping 0.35wt%)
The present embodiment crystal growth preparation process is substantially the same manner as Example 6, and difference is that proportioning raw materials is adjusted into K 2cO 3: Ta 2o 5: Nb 2o 5=1.2:0.3:0.7, Fe 2o 3content is adjusted into 2.8 grams, and crystal sintering temperature is adjusted into 1040 ° of C, and the crystal temperature of sowing is adjusted into 1145 ° of C, and growth temperature is adjusted into 1135 ~ 1145 ° of C; Crystal processing mode is identical with embodiment 1.
Embodiment 9:Fe:KTa 0.55nb 0.45o 3(Fe doping 0.1wt%)
The present embodiment crystal growth preparation process is substantially the same manner as Example 6, and difference is that proportioning raw materials is adjusted into K 2cO 3: Ta 2o 5: Nb 2o 5=1.1:0.23:0.77, Fe 2o 3content is adjusted into 0.85 gram, and crystal sintering temperature is adjusted into 1000 ° of C, and the crystal temperature of sowing is adjusted into 1120 ° of C, and growth temperature is adjusted into 1115 ~ 1125 ° of C; Crystal processing mode is identical with embodiment 6.
Embodiment 10: the capacitance of the M:KTN wafer that the present embodiment employing LCR bridge measurement embodiment 1 ~ 9 grows, calculate relative permittivity according to electric capacity, and determine the Curie temperature of each component crystal according to the variation of dielectric constant with temperature (be situated between temperature spectrum), and the specific inductivity of doped crystal in the present invention is compared with the not doping KTN crystal of same component, measurement of correlation result and experimental result see the following form 1.The present embodiment adopts the X section of embodiment 1 ~ 9 doping KTN crystal, and sample size is a × b × c=3mm ×2mm ×6mm, electrode end surface is (010) face, i.e. 3mm ×6mm end face,, thickness of sample 2mm, table 1 is for each sample is in the measured maximum dielectric constant of crystal vicinity of Curie temperatures and the secondary electro-optic coefficient value of answering in contrast.Contrast through the KTN crystal of ion doping and the crystal of undoped and can find, the secondary electro-optic coefficient of doped crystal is generally higher than pure KTN crystal, and surface ion doping can improve the electrooptic effect of KTN crystal really.
The electro-optical properties contrast of table 1. different sorts and concentration ion doping KTN crystal
Figure 176412DEST_PATH_IMAGE003

Claims (7)

1. there is formula M: KTa 1-xnb xo 3electro-optic crystal, crystal composition Nb content is 0.33≤ x≤ 0. 5, Curie temperature is positioned at-15 ~ 90 ° Cbetween, the above crystal of Curie temperature is Emission in Cubic, m3m point group; Curie temperature is Tetragonal below, 4mm point group.
2. electro-optic crystal as claimed in claim 1, is characterized in that M is Fe, Cu, and Co, Ni, and doping weight percent is 0 ~ 0.5 wt %.
3. a M:KTa 1-xnb xo 3the preparation method of crystal, with K 2cO 3, Nb 2o 5, Ta 2o 5for raw material, CuO, CoO, NiO and Fe 2o 3for dopant ion, adopt Czochralski grown, comprise the steps: that (1) is according to crystal composition, select batching according to KT-KN sosoloid phasor, through twice sintering, obtain M:KTN polycrystal, wherein dopant ion once and between double sintering is adding; (2) growing crystal in single crystal pulling stove; Heating member is platinum crucible, and growth atmosphere is air atmosphere; 1150 ~ 1250 ° of C materials, growing crystal between 1110 ~ 1200 ° of C, through the neck-shouldering of sowing-receive-wait the processes such as neck growth, obtains M:KTN crystal, growth cycle 5 ~ 10 days; (3) after crystal growing process finishes, be down to room temperature with suitable rate of temperature fall, take out crystal.
4. the preparation method of M:KTN crystal as claimed in claim 3, is characterized in that proportioning raw materials K 2cO 3: (Nb 2o 5+ Ta 2o 5) according to mol ratio (1.1 ~ 1.2): 1 weighs, and dopant ion oxide compound adds CuO, CoO, NiO or Fe according to 0 ~ 0.5% of raw material total mass 2o 3.
5. the growth method of M:KTN crystal as claimed in claim 3, the pull rate that it is characterized in that crystal growth is 0.25 ~ 0.5 milli m/h, crystalline substance turns 4 ~ 10 revs/min.
6. the process of growth of M:KTN crystal as claimed in claim 3, the rate of temperature fall while it is characterized in that in crystal temperature-fall period through Curie temperature is 1 ~ 2 ° of C/ hour.
7. an application for M:KTN crystal claimed in claim 1, its temperature limit is above 1 ~ 5 ° of C of Curie temperature.
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CN108521070A (en) * 2018-04-09 2018-09-11 山东省科学院新材料研究所 A kind of low voltage drive electro-optic Q switch based on tetragonal phase potassium tantalate-niobate crystal
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CN111323932A (en) * 2018-12-14 2020-06-23 青岛海信激光显示股份有限公司 Speckle eliminating device and projection display device
CN110230099A (en) * 2019-04-28 2019-09-13 山东省科学院新材料研究所 A kind of high dielectric constant potassium tantalate-niobate crystal preparation method
CN115974163A (en) * 2022-12-23 2023-04-18 山东省科学院新材料研究所 Zinc and titanium co-doped bismuth ferrite film and preparation method thereof
CN116041061A (en) * 2022-12-27 2023-05-02 山东省科学院新材料研究所 Potassium tantalate niobate ceramic and preparation method thereof
CN116041061B (en) * 2022-12-27 2023-12-26 山东省科学院新材料研究所 Potassium tantalate niobate ceramic and preparation method thereof

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