CN105586638A - Preparation method of potassium and lead niobate piezoelectric monocrystal - Google Patents
Preparation method of potassium and lead niobate piezoelectric monocrystal Download PDFInfo
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- CN105586638A CN105586638A CN201610129276.9A CN201610129276A CN105586638A CN 105586638 A CN105586638 A CN 105586638A CN 201610129276 A CN201610129276 A CN 201610129276A CN 105586638 A CN105586638 A CN 105586638A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/30—Niobates; Vanadates; Tantalates
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/14—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method characterised by the seed, e.g. its crystallographic orientation
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/02—Production of homogeneous polycrystalline material with defined structure directly from the solid state
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
Abstract
The invention discloses a preparation method of a potassium and lead niobate piezoelectric monocrystal. The method comprises the steps that a potassium and lead niobate polycrystal material synthesized at first is pressed into a compact cylindrical material block, high-quality potassium and lead niobate monocrystals in different directions are selected as seed crystals, the seed crystals are placed into the well portion at the bottom of a crucible, then the material block is placed into the crucible to be located at the high temperature area inside a hearth, the hearth temperature is controlled to be 1360-1390 DEG C, the solid-liquid interface temperature gradient is 6-10 DEG C/cm, the temperature is preserved for 3-7 h to enable polycrystal powder to be sufficiently fused, and the crucible lowering speed is 0.2-0.5 mm/h; after all the raw materials are crystallized, the crucible is made to be located at the hearth constant-temperature area, the temperature is preserved at the temperature of 1000-1200 DEG C, then the temperature is slowly decreased at the speed of 30-50 DEG C/h to reach the room temperature, the crystal is taken out, and therefore the light yellow potassium and lead niobate piezoelectric monocrystal is obtained. Growth of the high-quality potassium and lead niobate monocrystal is achieved, the monocrystal preparation difficulty is lowered, and the yield of the potassium and lead niobate monocrystal is greatly improved.
Description
Technical field
The invention belongs to physics field, relate to a kind of piezoelectric monocrystal, is the plumbous piezoelectric monocrystal of a kind of potassium niobate specificallyPreparation method.
Background technology
Phase at the end of the sixties in last century, surface acoustic wave (SAW) grows up gradually and becomes a kind of emerge science technology, and it isThe science that ultrasonics and electronics combine. Because SAW device has been realized miniaturization and multifunction, therebyRadar, navigation, electronics and identification field are widely applied. For SAW device, there are two important parameters,One is the time delay temperature coefficient relevant to its stability, and another is the electromechanical coupling factor relevant to its efficiency. Commonly useSubstrate material is lithium niobate monocrystal and α quartz, but the temperature coefficient of lithium niobate monocrystal is poor, the electromechanical coupling factor phase of α quartzBe on duty, this has brought serious problem to effective use of device. Tungsten bronze (T.B) is that ferro-electricity single crystal is because having good lightThe advantage such as cut type and high electromechanical coupling factor that electricity, thermoelectricity, piezoelectric property, time delay temperature coefficient are zero, and obtain people'sExtensive concern, that wherein electromechanical coupling factor is the highest is potassium niobate lead (Pb2KNb5O15) monocrystalline.
The plumbous monocrystalline of potassium niobate is a kind of novel piezoelectric monocrystalline growing up, and is also up-and-coming surface acoustic wave (SAW)The substrate material of device. In the last few years, lot of domestic and foreign university, research institution had carried out cubic blue steel structure potassium niobate leadThe growth of monocrystalline and application study. First T.Yamada etc. the have utilized Czochralski grown plumbous monocrystalline of potassium niobate, but because crucible isOpen, lead oxide is easy to volatilization at 1200 DEG C and causes solute segregation, can not make uniform stoichiometric(al) potassium niobate leadMonocrystalline, and still there is the defect such as crackle and twin in the monocrystalline growing. The people such as P.K.Pandey find again top-seeded solution growthWhile preparing the plumbous monocrystalline of potassium niobate, although crystal composition segregation is little, Binding, on sidewall of crucible, is difficult to it to draw from meltGo out. Visible, these growing methods are difficult to solve a difficult problem prepared by the plumbous piezoelectric monocrystal of high-quality potassium niobate.
Bridgman-Stockbarger method because of the crucible, crucible shape that use sealing as requested variable, temperature gradient of solid-liquid interface and underReduction of speed rate is widely used preparation some extremely difficult preparations according to many merits such as actual conditions regulation and control, many high efficiency of a stoveMonocrystalline, such as lithium tetraborate single crystal, relaxor ferroelectric monocrystal etc. Within 1999, Shanghai Inst. of Silicate, Chinese Academy of Sciences model generation horse is taughtWith<110>orientation seed crystal, temperature gradient of solid-liquid interface is set to 10 ~ 15 DEG C, utilizes Bridgman-Stockbarger method successfully to prepare high-qualityThe plumbous piezoelectric monocrystal of potassium niobate, but use<001>and<when 100>orientation seed crystal, the potassium niobate lead piezoelectric monocrystal growing stillOccur defects i.e.cracks, this is because temperature field is stable not, makes the vibration that Fast Growth causes easily destroy solid liquid interface temperatureDegree gradient, growth technique is better optimized simultaneously, makes crystal be easy to falling because of the anisotropy of thermal coefficient of expansionIn temperature process, there is crackle.
Adopt czochralski method, top seed crystal to plant the plumbous monocrystalline of potassium niobate that the method such as brilliant method, conventional crucibles descent method is prepared, depositLeak material, component macrosegregation, crystal at difficulty inoculation, crucible and contain the problem such as crackle and wrappage, yield rate only less than30%。
Summary of the invention
For above-mentioned technical problem of the prior art, the invention provides the preparation side of the plumbous piezoelectric monocrystal of a kind of potassium niobateMethod, the preparation method of the plumbous piezoelectric monocrystal of described this potassium niobate will solve the plumbous piezoelectricity of potassium niobate prepared by the method for prior artMonocrystalline exists difficult inoculation, crucible leakage material, component macrosegregation, crystal to contain the technical problem of crackle and parcel.
The preparation method who the invention provides the plumbous piezoelectric monocrystal of a kind of potassium niobate, comprises the steps:
1) step of a synthesis material piece: weigh PbO, be dried 1 ~ 3 hour in the air atmosphere of 550 ~ 650 DEG C; Treat natureAfter cool to room temperature, take out PbO, after fully grinding, then powder is placed in to dry 1 ~ 3 hour of the air atmosphere of 550 ~ 650 DEG C;Then by dry PbO powder, K2CO3And Nb2O5Weigh by mole mass ratio 4:1:5, under absolute alcohol environment, fully grindMill, mixes powder, and the powder obtaining is put into corundum crucible, is placed in Muffle furnace, at the air of 1100 ~ 1300 DEG CCalcination 5 ~ 15h in atmosphere after first sintering finishes, takes out after polycrystal material naturally cools to room temperature, after fully grinding,Powder is placed in Muffle furnace, in the air atmosphere of 1100 ~ 1300 DEG C, calcination 5 ~ 15 hours, after sintering, is down to for the second time againRoom temperature, obtains the plumbous polycrystal material of potassium niobate; Polycrystal material powder is pressed on hydraulic pressure or static pressure machine to fine and close bulk, obtains raw material block;
2) step of a crystal growth: select the plumbous monocrystalline of high-quality potassium niobate of different orientation as seed crystal, seed crystal is packed intoThe kind well position of crucible bottom, then packs raw material block into crucible, adjusts position, makes raw material block high-temperature region in burner hearth, stoveTemperature control is at 1360 ~ 1390 DEG C, and keeping temperature gradient of solid-liquid interface is 6 ~ 10 DEG C/cm, is incubated and within 3 ~ 7 hours, makes the plumbous polycrystalline of potassium niobateThe abundant melting of material raw material block, starts taking speed as 0.2 ~ 0.5mm/h the crucible that declines;
3) step of an annealing in process: after the whole crystallizations of raw material, make crucible in burner hearth flat-temperature zone, at 1000 ~ 1200 DEG CLower insulation 15 ~ 16h, then with 30 ~ 50 DEG C/h speed slow cooling to room temperature, take out crystal, can obtain light yellow potassium niobatePlumbous piezoelectric monocrystal.
Further, in preparation process (1) raw material block synthetic, the shape of raw material block is shaped as cylinder according to crucibleShape, rectangle or square.
Further, in the preparation process of step (2), described seed orientation is<110>,<001>or<100>sideTo, seed crystal shape is shaped as circle, rectangle or square according to crucible.
Further, at least two equivalent stations are set in Muffle furnace body, place at least two crucibles simultaneously, and prepareAt least two crystal.
Modified Bridgman-Stockbarger method is that plumbous potassium niobate synthetic solid-phase synthesis polycrystal material is pressed into fine and close block, its chiVery little and shape depends on the size and shape of crucible, and shape can be cylindric, rectangle or square shape etc., packs required crystalline substance intoIn the platinum crucible of body same size, move into descent method and prepare in the burner hearth of stove, and make raw material in Gao Qu, Control for Kiln Temperature is 1360~ 1390 DEG C, crucible fall off rate is 0.2 ~ 0.5mm/h, and temperature gradient of solid-liquid interface, between 6 ~ 10 DEG C, can be prepared light yellowThe plumbous monocrystalline of high-quality potassium niobate.
The present invention compares with prior art, and its technological progress is significant. The present invention has overcome czochralski method, top seed crystal is plantedDifficulty inoculation, the crucible that brilliant method and traditional Bridgman-Stockbarger method exist while preparing the plumbous monocrystalline of potassium niobate leak material, component macrosegregation,Crystal contains the problem such as crackle and wrappage, by adopting mullite fiber insulation material to increase temperature in crystal growing furnaceStability, airtight crucible reduces lead oxide volatilization, optimizes temperature gradient of solid-liquid interface, crucible fall off rate, annealing time etc.Technological parameter, has realized the growth of the plumbous monocrystalline of high-quality potassium niobate, has reduced single crystal preparation difficulty, has greatly improved potassium niobate leadThe yield rate of piezoelectric monocrystal. Have that equipment is simple simultaneously, the low batch production that is conducive to realize crystal of a stove fecund, cost etc. is excellentPoint.
Detailed description of the invention
Embodiment 1
Weigh PbO, the air atmosphere that is placed in inherent 600 DEG C of Muffle furnace is dried 2 hours; After naturally cooling to room temperature, take outPbO, the air atmosphere that again powder is placed in to inherent 600 DEG C of Muffle furnace after fully grinding is dried 2 hours. Again by high-purity(99.99%) dry PbO, K2CO3And Nb2O5Weigh by mole mass ratio 4:1:5, under absolute alcohol environment, fully grinding 10 is littleTime, powder is mixed, the powder obtaining is put into corundum crucible, and the air atmosphere that is placed in inherent 1200 DEG C of Muffle furnace burnsBurn 10h, i.e. compound first sintering. After polycrystal material naturally cools to room temperature, take out, fully regrind after 2 hours by powderEnd is placed in the air atmosphere calcination 10 hours of inherent 1200 DEG C of Muffle furnace, and compound sintering for the second time, is down to room temperature, obtainsThe plumbous polycrystal material of potassium niobate.
Embodiment 2
A preparation method for the plumbous piezoelectric monocrystal of potassium niobate, by plumbous high-purity (99.99%) potassium niobate polycrystal material, is pressed into fine and close cylinderShape material piece, packs in the platinum crucible of Φ 26mm, and it is Φ 10mm × 40mm<110 that crucible bottom is placed with size in advance>getTo seed crystal, be placed in appropriate location in improved Bridgman single crystal growing furnace, make raw material in high-temperature region, Control for Kiln Temperature is 1360DEG C, temperature gradient of solid-liquid interface, between 6 ~ 10 DEG C, is incubated and within 4 hours, makes the abundant melting of polycrystalline powder, under the speed with 0.5mm/hCrucible falls. After preparation finishes, crucible is placed in to flat-temperature zone in burner hearth, 1100 DEG C of annealing 15 hours, is down to room temperature, take out brilliantBody. Can prepare diameter is the plumbous monocrystalline of light yellow potassium niobate of Φ 25mm.
Embodiment 3
A preparation method for the plumbous piezoelectric monocrystal of potassium niobate, is pressed into fine and close cylinder by plumbous high-purity (99.99%) potassium niobate polycrystal materialShape material piece, packs in the platinum crucible of Φ 26mm, and it is Φ 10mm × 40mm<001 that crucible bottom is placed with size in advance>getTo seed crystal, be placed in appropriate location in improved Bridgman single crystal growing furnace, make raw material in high-temperature region, Control for Kiln Temperature is 1380DEG C, temperature gradient of solid-liquid interface, between 6 ~ 10 DEG C, is incubated and within 5 hours, makes the abundant melting of polycrystalline powder, under the speed with 0.3mm/hCrucible falls. After preparation finishes, crucible is placed in to flat-temperature zone in burner hearth, 1100 DEG C of annealing 15 hours, is down to room temperature, take out brilliantBody. Can prepare diameter is the plumbous monocrystalline of light yellow potassium niobate of Φ 25mm.
Embodiment 4
A preparation method for the plumbous piezoelectric monocrystal of potassium niobate, is pressed into fine and close cylinder by plumbous high-purity (99.99%) potassium niobate polycrystal materialShape material piece, packs in the platinum crucible of Φ 26mm, and it is Φ 10mm × 40mm<100 that crucible bottom is placed with size in advance>getTo seed crystal, be placed in appropriate location in improved Bridgman single crystal growing furnace, make raw material in high-temperature region, Control for Kiln Temperature is 1390DEG C, temperature gradient of solid-liquid interface, between 6 ~ 10 DEG C, is incubated and within 5 hours, makes the abundant melting of polycrystalline powder, under the speed with 0.3mm/hCrucible falls. After preparation finishes, crucible is placed in to flat-temperature zone in burner hearth, 1100 DEG C of annealing 16 hours, is down to room temperature, take out brilliantBody. Can prepare diameter is the plumbous monocrystalline of light yellow potassium niobate of Φ 25mm.
Embodiment 5
A preparation method for the plumbous piezoelectric monocrystal of potassium niobate, by the process conditions described in example 1,2,3, by<110>,<100>,<001 > etc. the crystal seed of different orientation is put into 8 platinum crucibles, prepares 8 plumbous monocrystalline of light yellow potassium niobate simultaneously.
Claims (4)
1. a preparation method for the plumbous piezoelectric monocrystal of potassium niobate, is characterized in that comprising the steps:
1) step of a synthesis material piece: weigh PbO, be dried 1 ~ 3 hour in the air atmosphere of 550 ~ 650 DEG C; Treat natureAfter cool to room temperature, take out PbO, after fully grinding, then powder is placed in to dry 1 ~ 3 hour of the air atmosphere of 550 ~ 650 DEG C;Then by dry PbO powder, K2CO3And Nb2O5Weigh by mole mass ratio 4:1:5, under absolute alcohol environment, fully grindMill, mixes powder, and the powder obtaining is put into corundum crucible, is placed in Muffle furnace, at the air of 1100 ~ 1300 DEG CCalcination 5 ~ 15h in atmosphere after first sintering finishes, takes out after polycrystal material naturally cools to room temperature, after fully grinding,Powder is placed in Muffle furnace, in the air atmosphere of 1100 ~ 1300 DEG C, calcination 5 ~ 15 hours, after sintering, is down to for the second time againRoom temperature, obtains the plumbous polycrystal material of potassium niobate; Polycrystal material powder is pressed on hydraulic pressure or static pressure machine to fine and close bulk, obtains raw material block;
2) step of a crystal growth: select the plumbous monocrystalline of potassium niobate of different orientation as seed crystal, at the bottom of packing seed crystal into crucibleThe kind well position of portion, then packs raw material block into crucible, adjusts position, makes raw material block high-temperature region in burner hearth, Control for Kiln TemperatureAt 1360 ~ 1390 DEG C, keeping temperature gradient of solid-liquid interface is 6 ~ 10 DEG C/cm, is incubated and within 3 ~ 7 hours, makes the plumbous polycrystal material raw material of potassium niobateThe abundant melting of piece, starts taking speed as 0.2 ~ 0.5mm/h the crucible that declines;
3) step of an annealing in process: after the whole crystallizations of raw material, make crucible in burner hearth flat-temperature zone, at 1000 ~ 1200 DEG CLower insulation 15 ~ 16h, then with 30 ~ 50 DEG C/h speed slow cooling to room temperature, take out crystal, can obtain light yellow potassium niobatePlumbous piezoelectric monocrystal.
2. the preparation side of the plumbous piezoelectric monocrystal of a kind of potassium niobate as claimed in claim 1, is characterized in that: in preparation process (1)In raw material block synthetic, the shape of raw material block is shaped as cylindrical, rectangle or square according to crucible.
3. the preparation method of the plumbous piezoelectric monocrystal of a kind of potassium niobate as claimed in claim 1, is characterized in that: in step (2)In preparation process, described seed orientation is<110>,<001>or<100>direction, seed crystal shape is shaped as circle according to crucibleShape, rectangle or square.
4. the preparation method of the plumbous piezoelectric monocrystal of a kind of potassium niobate as claimed in claim 1, is characterized in that: in Muffle furnace body, establishPut at least two equivalent stations, place at least two crucibles simultaneously, and prepare at least two crystal.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108330542A (en) * | 2018-02-02 | 2018-07-27 | 上海应用技术大学 | A kind of bromine silicic acid leading crystal and preparation method thereof |
| CN112899780A (en) * | 2021-01-20 | 2021-06-04 | 吉林大学 | Directional growth method of relaxation ferroelectric single crystal lead niobate zincate-lead titanate |
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| CN108330542A (en) * | 2018-02-02 | 2018-07-27 | 上海应用技术大学 | A kind of bromine silicic acid leading crystal and preparation method thereof |
| CN112899780A (en) * | 2021-01-20 | 2021-06-04 | 吉林大学 | Directional growth method of relaxation ferroelectric single crystal lead niobate zincate-lead titanate |
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