CN102925959A - Novel growth technology of relaxation ferroelectric monocrystal PIMNT (Lead Magnesium/Indium Niobate-Lead Titanate) - Google Patents
Novel growth technology of relaxation ferroelectric monocrystal PIMNT (Lead Magnesium/Indium Niobate-Lead Titanate) Download PDFInfo
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Abstract
The invention discloses a novel growth technology of relaxation ferroelectric mono-crystal PIMNT by using a Bridgman-Stockbarger method, belonging to the technical field of mono-crystal growth. The novel growth technology of the relaxation ferroelectric mono-crystal PIMNT comprises the steps of: regarding high-purity PbO, Nb2O5, In2O3, TiO2 and 4MgCO3.Mg(OH)2.4H2O as initial raw materials to prepare a PIMNT polycrystal material through a precursor step-by-step synthesis method, wherein the chemical constitution is xPb(In1/2Nb1/2)O3-yPb(Mg1/2Nb2/3)O3-(1-x-y)PbTiO3, where x=0.24-0.26, and y=0.43-0.45; selecting high-quality seed crystal in a [110], [111] or [001] crystallographic direction; adopting a single-layer or double-layer seamless platinum crucible to contain the seed crystal and a material ingot; putting the crucible after being sealed in a mono-crystal growth furnace; controlling the temperature of the furnace at 1350-1400 DEG C; adjusting the position of the crucible to enable the material ingot to be welded with the top part of the seed crystal so as to form a steady solid-liquid interface with a temperature gradient of 20-50 DEG C; and growing the mono-crystal at a dropping speed of the crucible of less than 1 mm/h to obtain a high-quality and large-size PIMNT mono-crystal. The novel growth technology of the relaxation ferroelectric mono-crystal PIMNT, disclosed by the invention, has the advantages of overcoming a leakage phenomenon of a high-temperature lead-rich melt, avoiding volatilization of components of the melt, and particularly lead oxide steam, efficiently solving a poly-crystallized growth problem of a solid solution with composition complexity, and being suitable for growing high-quality and large-size PIMNT mono-crystals in batches.
Description
Technical field
The invention belongs to the Crystal Growth Technique field.The PIMNT monocrystalline is the high-performance relaxor ferroelectric crystalline material of in recent years latest find, and the PIMNT of accurate homotype phase boundary composition has very high piezoelectric constant, with traditional piezoelectric PZT ceramic phase ratio, and its piezoelectric constant d
33, electromechanical coupling factor K
33From about 500pC/N and 60%, bring up to respectively about 2000pC/N and 90%, its strain is up to more than 1%, be about 0.1% high 1 order of magnitude of piezoelectric than common strain, this material has extremely important using value in high-tech sectors such as medical ultrasound image, sonar technique, ultrasonic motor, non-destructive test(ing)(NDT)s.Adopt the technology of the present invention can grow the high quality large size PIMNT monocrystalline that satisfies practical needs.
Background technology
The nineties is since the later stage, the material supply section scholar has successively found series high-performance relaxor ferroelectric monocrystal material, such as lead zinc niobate-lead titanate (PZNT), PMN-PT (PMNT), lead niobate lead indate-lead-lead titanate (PINT) etc., the serial relaxor ferroelectric monocrystal material of accurate homotype phase boundary composition all has excellent piezoelectric property, its piezoelectric constant d
33, electromechanical coupling factor K
33Can be up to about 2000pC/N and 90%, its strain is up to more than 1%, be considered to the important breakthrough in piezoelectric field since half a century, such monocrystal material has broad prospect of application in acoustic-electric switch technology fields such as medical ultrasound image, sonar technique, ultrasonic motor, non-destructive test(ing)(NDT)s, and the PMNT monocrystalline has obtained the short run application in relevant piezoelectric device field so far.
In the relaxor ferroelectric monocrystal material of having reported, the PZNT monocrystalline must be grown from the system solid solution that adds a large amount of solubility promoter PbO, the burnt green stone crystallization phases of the normal association of the melt growth process of PINT monocrystalline, and all being difficult to grow obtains large-size monocrystalline with practical value; The PMNT monocrystalline can be directly forms the melt from metering and grow out, relatively is easy to grow obtain large-size monocrystalline with practical value, but the phase transition temperature T of PMNT monocrystalline
R/tWith Curie temperature T
cOnly be respectively 60-95 ℃ and 130-170 ℃, the phase transition temperature that it is lower and Curie temperature still are difficult to satisfy the application requiring of superpower piezoelectric device.
Recent domestic material scholar has reported a kind of novel relaxor ferroelectric monocrystal PIMNT in succession, and its chemical constitution is xPb (In
1/2Nb
1/2) O
3-y Pb (Mg
1/2Nb
2/3) O
3-(1-x-y) PbTiO
3, belonging to the ternary solid solution monocrystalline of perovskite structure, its density of material is 8.15-8.20g/cm
3The PIMNT monocrystalline has with the similar crystallization characteristic of PMNT monocrystalline, can directly form the melt from metering to grow out, and its crystal admixtion needn't add fusing assistant PbO, even can adopt the PMNT crystal to carry out oriented growth as seed crystal; The PIMNT crystal also has the fusing point more lower slightly than PMNT, and its single crystal growing temperature also can reduce about 20 ℃, helps to slow down rich plumbous melt to the erosion action of crucible equipment.
The sosoloid monocrystal that PIMNT monocrystalline system grows from the rich plumbous melt of polycomponent, there is a following inherent technology difficult problem in its single crystal growth process: the plumbous oxide content of (1) PIMNT polycrystal is quite high, the plumbous melt of this richness produces than the vigorous erosion effect the metal platinum crucible, cause the platinum crucible wall small hole or microcrack to occur, so that melt generation seepage in various degree in the crucible; (2) the comparatively complicated ternary solid solution compound of PIMNT crystal system composition is easy to form ceramic polycrystalline material through the high temperature solid-phase sintering process, and its single crystal growth process is easy to occur the polycrystallization growth and is difficult to obtain monocrystal material; (3) there is intrinsic solute segregation in this lead base sosoloid monocrystal growth, correspondingly causes its monocrystalline proembryo to change continuously along axial performance, becomes the obvious inhomogeneity restraining factors of material property that affect.
The invention provides the Bridgman-Stockbarge method for growing technique of PIMNT monocrystalline, by the synthetic PIMNT polycrystal ingot of high-temperature solid phase reaction method, adopt the special individual layer of metal platinum plate or double-deck seamless crucible, under the crucible air tight condition, carry out the PIMNT single crystal growing.This technique can effectively be avoided the particularly volatilization of plumbous oxide steam of bath composition, is conducive to reduce the solute segregation of single crystal growth process; Adopt the seed crystal of [110] or [111] or [001] crystallographic direction to carry out the oriented monocrystalline growth, can effectively avoid contingent polycrystallization growth, in addition, adopt the multi-work-station monocrystal growing furnace can many monocrystalline of every secondary growth, this technique can be applied in batches growing high-quality large size PIMNT monocrystalline.
Summary of the invention
Technical process of the present invention is shown in Figure of description 1, and its main contents are described below:
1, polycrystal is synthetic
(1) oxide compound PbO, the Nb of employing 99.9% above purity
2O
5, In
2O
3, 4MgCO
3Mg (OH)
24H
2O and TiO
2Be starting raw material, prepare the PIMNT polycrystal by the presoma step synthesis, namely synthesize respectively first precursor compound InNbO
4And MgNb
2O
6, resynthesis ternary solid solution PIMNT polycrystal.
(2) by stoichiometric ratio preparation 4MgCO
3Mg (OH)
24H
2O and Nb
2O
5Compound, 1100 ℃ of lower sintering 6 hours with synthetic MgNb
2O
6Press n (In
2O
3): n (Nb
2O
5The molar ratio of)=1: 1 preparation compound, 1100 ℃ of lower sintering 6 hours with synthetic InNbO
4
(3) according to the stoichiometric composition that fits to the PIMNT polycrystal, with PbO, InNbO
4, MgNb
2O
6, TiO
2Ground and mixed in addition fully 850 ℃ of lower sintering 4 hours, synthesizes the brown color PIMNT polycrystal ingot of perovskite structure with the mixture that is pressed into the material ingot.
(4) chemical constitution of institute's synthesised polycrystalline material is xPb (In
1/2Nb
1/2) O
3-yPb (Mg
1/2Nb
2/3) O
3-(1-x-y) PbTiO
3, x=0.24～0.26 wherein, y=0.43～0.45 adopts this polycrystal through optimizing to form, can be so that institute's growing single-crystal proembryo have comparatively desirable performance perameter distributes, the tripartite phase crystallization section of the piezoelectric property that especially obtains more to grow tall.
2, platinum crucible is made
(1) smelting metal platinum in high frequency furnace is pressed into metal platinum approximately 0.4～1.0 millimeter sheet material of thickness again; Make the size of crucible according to drawing up and shear platinum sheet material, institute's shear material is wrapped in red copper mould outer wall, elder generation's point of application soldering method welding forming crucible, use argon arc welding method again so that weld seam fully makes up, at last the shaping crucible is fixed on the lathe, crucible integral body especially weld seam is carried out squeezing shaping, to produce the smooth seamless crucible of surfaces externally and internally.
(2) for the requirement of single crystal growing to the crucible erosion-resisting characteristics, the present invention produces two types seamless platinum crucible, i.e. individual layer crucible or double crucible.Adopt thicker platinum board making to go out the individual layer platinum crucible of wall thickness 0.6～1.0mm, perhaps adopt two crucibles producing respectively wall thickness 0.3～0.5mm than light sheet, with the individual layer thin-walled crucible sleeve of two size match altogether, the double-deck seamless crucible of made more is conducive to avoid contingent melt leakage.
(3) adopt above-mentioned making method can produce equal diameter or non-isodiametric round shape platinum crucible, its underpart is used for installing seed crystal with the growth of guiding oriented monocrystalline.Seed crystal is installed on the small diameter bottom of non-equal diameter crucible, and the polycrystal splendid attire just can be used the guiding of small diameter seed crystal and grow the larger diameter monocrystalline in the larger diameter middle and upper part.
3, single crystal growing
(1) obtains the PIMNT seed crystal by spontaneous nucleation growth in advance, choose the cylindrical seed crystal that even complete monocrystalline is processed into diameter 10～75mm, longitudinal length is 40～50mm, and the ratio of growing single-crystal and the cross-sectional area of seed crystal is wanted less than 4 in its crystallographic direction [110] or [111] or [001].
(2) first seed crystal is installed on the crucible bottom, seed crystal should be close to sidewall of crucible, loads polycrystal in crucible top again, last sealing crucible top, to avoid that the bath composition volatilization occurs in the single crystal growth process, be conducive to the solute segregation that bath component is stablized and reduced institute's growing single-crystal in the crucible.
(3) crucible is put into the vitrified pipe appropriate location, made the seed crystal top mutually neat with temperature thermocouple, then the filling aluminum oxide powder puts into burner hearth with vitrified pipe in the gap of crucible and vitrified pipe, is placed on the mechanical lowering means; Furnace temperature is risen to the control temperature, and automatic heat preserving is in 1350～1400 ℃, again crucible moved on progressively, be adjusted at last suitable height, make the seed crystal top realize welding with crucible top polycrystal.
(4) with crucible fixed position insulation 4～6 hours, then the stable solid-liquid interface take the formation temperature gradient as 20～50 ℃/cm makes crucible with less than 1mm/ hour speed slow decreasing, the PIMNT monocrystalline is just separated out from melt gradually.Single crystal growth process stops crucible decline process after finishing, and, to room temperature the monocrystalline proembryo is peeled off from crucible with 30～50 ℃/hour rate reduction furnace temperature, obtains oriental topaz look PIMNT monocrystalline.
(5) place annealing furnace to heat-treat obtaining PIMNT monocrystalline, annealing furnace is warming up to 850～900 ℃ with 50 ℃/hour speed, in oxygen or air atmosphere, be incubated 6～12 hours, again with 50 ℃/hour speed cool to room temperature.Annealed processing can be eliminated the crystal thermal stresses and reduce lattice defect, thereby obtains the oriental topaz look PIMNT monocrystalline of color even.
Description of drawings
Accompanying drawing 1 is PIMNT polycrystal synthesis flow.
Accompanying drawing 2 is PIMNT monocrystalline growing process flow process.
Accompanying drawing 3 is the used Bridgman-Stockbarge method single crystal growth furnace schematic diagram of the present invention.This system partly is comprised of growth furnace, temperature controller, temperature element and mechanical lowering means etc.The burner hearth of this growth furnace is divided into high-temperature zone, zone of transition and cold zone, the Si-Mo rod heating is adopted in the high-temperature zone, and cold zone utilizes waste heat to regulate temperature, and has thermal baffle to make upper and lower warm area separately, the thermograde of high and low warm area is all less, and the thermograde of transitional region is larger therebetween.In single crystal growth process, polycrystal melts in the high-temperature zone, and monocrystalline is in cold zone insulation and self-annealing, and solid-liquid interface is positioned at transitional region.By the accurate temperature controller control of WJK-100A furnace body temperature, adopting the Pt/Pt-10%Rh thermopair is temperature control and temperature element, and the cold junction of thermopair all is placed in the curling stone.In order to measure in real time the temperature variation of single crystal growth process, two pairs of temperature thermocouples are placed in the alumina ceramic tube, the hot junction of two pairs of thermopairs is at a distance of 100mm, and this vitrified pipe is used for supporting platinum crucible.The machinery lowering means is comprised of screw mandrel, stepper-motor and harmonic speed reducer, and the speed that crucible descends is by the single card microcomputer time variable control.Start mechanical lowering means, crucible is with the given pace slow decreasing, and monocrystalline is separated out from melt gradually from bottom to top.Adopt many crucibles monocrystal growing furnace, every growth furnace many monocrystalline of at every turn can growing.
Accompanying drawing 4 is by adopting the present invention to be grown
The PIMNT monocrystalline.
Accompanying drawing 5 is by adopting the present invention to be grown
The PIMNT monocrystalline.
Embodiment
Embodiments of the invention are listed below:
(1) adopt the platinum plate of wall thickness 0.7mm to be processed into the cylindric crucible of non-equal diameter, its underpart volume is
Upper volume is
The centre is funnel-form.To be orientated [110], size
Seed crystal be installed on the crucible bottom, load again polycrystal, then sealing crucible two ends toward the crucible middle and upper part.In single crystal growth process, growth furnace is controlled in 1380～1390 ℃, regulate first crucible to the appropriate location, make the fusing of polycrystal and seed crystal top, the formation temperature gradient is the stable solid-liquid interface of 30 ℃/cm, is incubated after 4 hours, and crucible is descended with 0.5mm/ hour speed.Single crystal growth process is down to room temperature with furnace temperature with 40～50 ℃/hour speed after finishing, and can obtain size and reach
Oriental topaz look complete PIMNT monocrystalline.
(2) adopt the platinum plate of wall thickness 1.0mm to be processed into the cylindric crucible of non-equal diameter, its underpart volume is
Upper volume is
The centre is funnel-form.To be orientated [111], size 24.8 * 50mm
3Seed crystal be installed on the crucible bottom, load again polycrystal, then sealing crucible two ends.Control for Kiln Temperature in 1390～1400 ℃, is regulated crucible to the appropriate location, make the fusing of raw material and seed crystal top, the thermograde of solid-liquid interface is 40 ℃/cm, be incubated after 5 hours, makes crucible with 0.4mm/ hour speed decline.Single crystal growth process is down to room temperature with furnace temperature with 30～40 ℃/hour speed after finishing, and can obtain size and reach
Oriental topaz look complete PIMNT monocrystalline.
(3) according to example 1,2 described processing condition, the seed crystal that will be orientated [110] or [111] is put into 3 crucibles, carries out single crystal growing in three station growth furnace, 3 the PIMNT monocrystalline of can growing simultaneously.
Claims (5)
1. the Bridgman-Stockbarge method for growing technique of novel relaxor ferroelectric monocrystal PIMNT comprises the steps such as polycrystal is synthetic, single crystal growing, it is characterized in that:
(1) with 99.9% above purity PbO, Nb
2O
5, In
2O
3, 4MgCO
3Mg (OH)
24H
2O and TiO
2Be starting raw material, synthesize first presoma InNbO by high-temperature solid phase reaction method
4And MgNb
2O
6, resynthesis ternary solid solution PIMNT polycrystal, its chemical constitution is xPb (In
1/ 2Nb
1/ 2) O
3-yPb (Mg
1/2Nb
2/3) O
3-(1-x-y) PbTiO
3
(2) adopt individual layer or double-deck platinum crucible splendid attire seed crystal and material ingot, sealed crucible is placed in the monocrystal growing furnace, the control furnace temperature is in 1350～1400 ℃, regulate bushing position and make material ingot and the welding of seed crystal top, the formation temperature gradient is 20～50 ℃/centimetre stable solid-liquid interface, then carries out single crystal growing with the crucible fall off rate less than 1 millimeter/hour.
2. PIMNT monocrystalline growing process according to claim 1, the chemical constitution that it is characterized in that the polycrystal that adopts is xPb (In
1/2Nb
1/2) O
3-yPb (Mg
1/2Nb
2/3) O
3-(1-x-y) PbTiO
3, x=0.24～0.26 wherein, y=0.43～0.45 adopts this polycrystal through optimizing to form, can be so that institute's growing single-crystal proembryo have comparatively desirable performance perameter distributes, the tripartite phase crystallization section of the piezoelectric property that especially obtains more to grow tall.
3. PIMNT monocrystalline growing process according to claim 1, it is characterized in that adopting individual layer or double-deck platinum crucible to carry out single crystal growing, the metal platinum sheet material of this platinum crucible employing 0.4～1.0mm of system thickness, being aided with extrusion process by spot welding with the fire weldering is made, the made crucible can be equal diameter or non-equal diameter round shape, its underpart is used for suitable specification seed crystal is installed, and the polycrystal splendid attire is in the crucible middle and upper part.
4. PIMNT monocrystalline growing process according to claim 1 is characterized in that adopting the seed crystal of [110] or [111] or [001] crystallographic direction to grow to realize oriented monocrystalline, can effectively avoid contingent polycrystallization growth; The seed crystal that adopts is the cylindrical monocrystalline of 10～75mm diameter, and its longitudinal length is 40～50mm, wants the ratio of growing single-crystal and the cross-sectional area of seed crystal less than 4.
5. PIMNT monocrystalline growing process according to claim 1, it is characterized in that under the crucible air tight condition, carrying out the PIMNT single crystal growing, can effectively avoid the particularly volatilization of plumbous oxide steam of bath composition, thereby the composition that reduces monocrystalline proembryo due to the effect of segregation changes, and is conducive to grow high quality large size PIMNT monocrystalline.
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Application publication date: 20130213 |