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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- CN102925959A CN102925959A CN 201210403334 CN201210403334A CN102925959A CN 102925959 A CN102925959 A CN 102925959A CN 201210403334 CN201210403334 CN 201210403334 CN 201210403334 A CN201210403334 A CN 201210403334A CN 102925959 A CN102925959 A CN 102925959A
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- 230000012010 growth Effects 0.000 title claims abstract description 34
- 238000005516 engineering process Methods 0.000 title description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title 1
- 229910052738 indium Inorganic materials 0.000 title 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 title 1
- 229910052749 magnesium Inorganic materials 0.000 title 1
- 239000011777 magnesium Substances 0.000 title 1
- 239000013078 crystal Substances 0.000 claims abstract description 63
- 238000000034 method Methods 0.000 claims abstract description 40
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 38
- 230000008569 process Effects 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 20
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 11
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000006104 solid solution Substances 0.000 claims abstract description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 4
- YEXPOXQUZXUXJW-UHFFFAOYSA-N lead(II) oxide Inorganic materials [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims description 8
- 239000012071 phase Substances 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
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- 150000003057 platinum Chemical class 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract description 2
- 229910019440 Mg(OH) Inorganic materials 0.000 abstract 1
- 239000010410 layer Substances 0.000 abstract 1
- 229910000464 lead oxide Inorganic materials 0.000 abstract 1
- 239000002356 single layer Substances 0.000 abstract 1
- 239000007858 starting material Substances 0.000 abstract 1
- WKBPZYKAUNRMKP-UHFFFAOYSA-N 1-[2-(2,4-dichlorophenyl)pentyl]1,2,4-triazole Chemical compound C=1C=C(Cl)C=C(Cl)C=1C(CCC)CN1C=NC=N1 WKBPZYKAUNRMKP-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000011031 topaz Substances 0.000 description 4
- 229910052853 topaz Inorganic materials 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 101000687727 Homo sapiens Transcriptional regulator PINT87aa Proteins 0.000 description 2
- 102100024797 Transcriptional regulator PINT87aa Human genes 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910006295 Si—Mo Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 239000003638 chemical reducing agent Substances 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
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- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了新型弛豫铁电单晶PIMNT的坩埚下降法生长工艺，该发明属于单晶生长技术领域。以高纯度PbO、Nb2O5、In2O3、TiO2和4MgCO3·Mg(OH)2·4H2O为起始原料，通过前驱体分步合成法制备PIMNT多晶料，其化学组成为xPb(In1/2Nb1/2)O3-yPb(Mg1/2Nb2/3)O3-(1-x-y)PbTiO3，其中x＝0.24～0.26，y＝0.43～0.45。选用[110]或[111]或[001]结晶学方向的优质籽晶，采用单层或双层无缝铂坩埚盛装籽晶和料锭，将坩埚密封后置于单晶生长炉中，控制炉温于1350～1400℃，调节坩埚位置使料锭与籽晶顶部熔接，形成温度梯度为20～50℃/cm的稳定固液界面，以小于1mm/小时的坩埚下降速率进行单晶生长，可获得高质量大尺寸PIMNT单晶。该工艺能够克服高温富铅熔体的渗漏现象，避免熔体成分特别是氧化铅蒸气的挥发，有效解决组成复杂的固溶体多晶化生长问题，适用于批量生长高质量大尺寸PIMNT单晶。The invention discloses a crucible drop method growth process of novel relaxor ferroelectric single crystal PIMNT, which belongs to the technical field of single crystal growth. Using high-purity PbO, Nb 2 O 5 , In 2 O 3 , TiO 2 and 4MgCO 3 ·Mg(OH) 2 ·4H 2 O as starting materials, the PIMNT polycrystalline material was prepared by stepwise synthesis of precursors. The composition is xPb(In 1/2 Nb 1/2 )O 3 -yPb(Mg 1/2 Nb 2/3 )O 3 -(1-xy)PbTiO 3 , where x=0.24～0.26, y=0.43～0.45 . Select high-quality seed crystals of [110] or [111] or [001] crystallographic direction, use a single-layer or double-layer seamless platinum crucible to hold the seed crystals and ingots, seal the crucible and place it in a single crystal growth furnace. Furnace temperature is 1350-1400°C, adjust the position of the crucible so that the ingot and the top of the seed crystal are fused to form a stable solid-liquid interface with a temperature gradient of 20-50°C/cm, and the crucible descending rate is less than 1mm/hour for single crystal growth. High-quality and large-size PIMNT single crystals can be obtained. This process can overcome the leakage phenomenon of high-temperature lead-rich melt, avoid the volatilization of melt components, especially lead oxide vapor, and effectively solve the problem of polycrystalline growth of solid solution with complex composition. It is suitable for batch growth of high-quality and large-sized PIMNT single crystals.
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210403334 CN102925959A (en) | 2012-10-14 | 2012-10-14 | Novel growth technology of relaxation ferroelectric monocrystal PIMNT (Lead Magnesium/Indium Niobate-Lead Titanate) |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210403334 CN102925959A (en) | 2012-10-14 | 2012-10-14 | Novel growth technology of relaxation ferroelectric monocrystal PIMNT (Lead Magnesium/Indium Niobate-Lead Titanate) |
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| Publication Number | Publication Date |
|---|---|
| CN102925959A true CN102925959A (en) | 2013-02-13 |
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| CN103866386A (en) * | 2014-03-04 | 2014-06-18 | 西安交通大学 | Preparation method of novel ternary piezoelectric crystal monophase material |
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| CN110318097A (en) * | 2019-07-25 | 2019-10-11 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of niobic acid gallium langasite single crystal |
| CN112831839A (en) * | 2021-01-07 | 2021-05-25 | 生物岛实验室 | A kind of preparation method of raw material for relaxor ferroelectric single crystal growth |
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