CN116905081A - Method for fast growth of single crystal by electric field assisted solid phase method - Google Patents
Method for fast growth of single crystal by electric field assisted solid phase method Download PDFInfo
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- CN116905081A CN116905081A CN202310928985.3A CN202310928985A CN116905081A CN 116905081 A CN116905081 A CN 116905081A CN 202310928985 A CN202310928985 A CN 202310928985A CN 116905081 A CN116905081 A CN 116905081A
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- electric field
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- phase method
- single crystal
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- 239000013078 crystal Substances 0.000 title claims abstract description 72
- 230000005684 electric field Effects 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000010532 solid phase synthesis reaction Methods 0.000 title claims abstract description 27
- 239000000919 ceramic Substances 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 15
- 229910002367 SrTiO Inorganic materials 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 5
- 239000012071 phase Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 238000002490 spark plasma sintering Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009694 cold isostatic pressing Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Classifications
-
- 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
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
-
- 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
- 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
- C30B29/32—Titanates; Germanates; Molybdates; Tungstates
-
- 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
- C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
- C30B30/02—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions using electric fields, e.g. electrolysis
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention belongs to the technical field of single crystal growth by a solid phase method, and particularly relates to a method for rapidly growing single crystals by an electric field assisted solid phase method. The method can improve the growth speed of the single crystal on the basis of reducing the volatilization of elements of a complex system and enabling the components of the single crystal to be uniform and controllable.
Description
Technical Field
The invention belongs to the technical field of single crystal growth by a solid phase method, and particularly relates to a method for rapidly growing single crystals by an electric field-assisted solid phase method.
Technical Field
Single crystals have found widespread use in industrial production. Common single crystal growth techniques are liquid phase, gas phase and solid phase. Vapor phase methods typified by vapor deposition techniques are generally used for the production of thin film single crystals; the liquid phase method represented by Bridgman method is the most common method for preparing single crystals, and the technology needs to heat to the melting point, has high temperature, is easy to generate uneven component distribution or volatile component with low melting point, and is not beneficial to the single crystal growth of a complex component system. The solid phase method single crystal growth realizes single crystal solid phase growth by means of abnormal growth of crystal grains, and has low temperature and uniform components, but the single crystal growth speed of the technology is slower.
Therefore, increasing the rate of single crystal growth during the preparation of single crystals using the solid phase method is a problem to be solved in the prior art.
Disclosure of Invention
The invention aims to provide a method for rapidly growing single crystals by using an electric field assisted solid phase method, which can improve the growth speed of the single crystals on the basis of reducing the volatilization of elements of a complex system and enabling the components of the single crystals to be uniform and controllable.
The invention aims at realizing the following technical scheme:
the invention provides a method for rapidly growing single crystals by using an electric field assisted solid phase method, which accelerates the growth speed of the single crystals by applying an electric field assisted heat treatment in the process of preparing the single crystals by using the solid phase method.
Further, the method comprises the following steps:
step 1: pressing and forming the single crystal template and the target crystal powder together to obtain a ceramic green body;
step 2: pre-sintering the ceramic green body in the step 1;
step 3: and (3) performing heat treatment on the ceramic green body subjected to presintered in the step (2) by adopting an electric field assisted sintering technology, so as to realize the rapid growth of single crystals.
Further, the single crystal template in the step 1 comprises SrTiO 3 、KTaO 3 Any single crystal template material including [100 ] in crystal phase]、[110]、[111]Any of which is included.
Further, the target crystal powder in the step 1 is SrTiO corresponding to the single crystal template 3 、K 0.5 Na 0.5 NbO 3 Any crystal powder.
Further, the pre-sintering temperature in the step 2 is 500-1100 ℃, and the pre-sintering time is 1-24h.
Further, the electric field assisted sintering technique in the step 3 is as follows:
serially connecting the green bodies into a circuit; then placing the green body in a heating furnace, heating to the temperature of the green body to a preset constant temperature, applying a preset constant electric field to the green body until a flash phenomenon occurs, converting a constant voltage state into a constant current state by a power supply after the flash phenomenon occurs, controlling the current density of the constant current state, keeping for a period of time under the current density, closing the power supply, closing the heating furnace, and reducing the temperature.
Furthermore, the electric field assisted sintering technology can apply a preset constant electric field to the green body while heating, and continuously heating until a flash phenomenon occurs.
Further, the preset constant temperature is 600-1100 ℃.
Further, the electric field strength of the preset constant electric field is 100V/cm-1000V/cm.
Further, the current density of the constant current state is 10mA/mm 2 -1000mA/mm 2 The holding time of the constant current state is 0.5h-240h, and the cooling mode is furnace-following cooling.
Further, the press forming in the step 1 includes, but is not limited to, compression molding, cold isostatic pressing, and the like.
The invention has the beneficial effects that:
the invention accelerates the growth speed of single crystal by solid phase method based on the characteristic of rapid mass transfer of substances under the assistance of critical electric field, and can improve the growth speed of single crystal on the basis of reducing the volatilization of elements of complex system and ensuring uniform and controllable single crystal components.
Drawings
FIG. 1 shows SrTiO obtained in example 1 3 Cross-sectional scanning electron micrographs of the samples;
FIG. 2 is a graph of K obtained in example 2 0.5 Na 0.5 NbO 3 Cross-sectional scanning electron micrographs of the samples.
Detailed Description
The following experimental examples and examples serve to further illustrate the invention but are not limited thereto.
Example 1
Electric field assisted SrTiO 3 The solid phase method single crystal growth comprises the following steps:
step 1: will [100 ]]SrTiO of crystal orientation 3 The single crystal template is embedded into SrTiO by a mould pressing mode 3 Obtaining ceramic green compact by the powder;
step 2: pre-sintering the ceramic green body at 1000 ℃ (500-1400 ℃ can be achieved) for 2h (1-24 h can be achieved) to obtain a ceramic preform;
step 3: placing the ceramic preform into an electric field auxiliary sintering furnace, connecting the electric field auxiliary sintering furnace in series, setting a heating rate of 10 ℃/min to heat to 1000 ℃ (600-1100 ℃), applying a direct current electric field of 250V/cm (100V/cm-1000V/cm) to two ends of the ceramic preform through a platinum wire, maintaining the electric field strength until flash firing occurs, converting the power supply from a constant voltage mode to a constant current mode, and controlling the current density to 100mA/mm 2 (10mA/mm 2 -1000mA/mm 2 Can be maintained for 30 minutes (0.5 h-240 h). And then turning off the direct current power supply, turning off the sintering furnace, and cooling the sample along with the furnace.
FIG. 1 shows SrTiO obtained in the present example 3 The cross-sectional scanning electron micrograph of the sample can be seen as SrTiO within 30 minutes with the assistance of an electric field 3 The single crystal grows to about 70 μm.
Example 2
Electric field assisted K 0.5 Na 0.5 NbO 3 The solid phase method single crystal growth comprises the following steps:
step 1: will [110 ]]KTaO of crystal orientation 3 The single crystal template is embedded into K by a mould pressing mode 0.5 Na 0.5 NbO 3 Obtaining ceramic green compact by the powder;
step 2: the ceramic green body is presintered for 10 hours (1-24 hours can be carried out) at 1080 ℃ (500-1100 ℃ can be carried out) furnace temperature to obtain a ceramic preform;
step 3: the ceramic preform is put into an electric field auxiliary sintering furnace, a series circuit is adopted, a direct current electric field of 300V/cm (100V/cm-1000V/cm can be applied to the two ends of the ceramic preform through a platinum lead, the sintering furnace is arranged under the continuous loading of the electric field to heat the sample,until flash firing occurs, the power supply is changed from a constant voltage mode to a constant current mode, a sintering furnace program is set at the moment to keep the furnace temperature unchanged, and the current density is controlled to be 20mA/mm 2 (10mA/mm 2 -1000mA/mm 2 All can be carried out, and the time is kept for 1 hour (all can be carried out for 0.5h-240 h). And then turning off the direct current power supply, turning off the sintering furnace, and cooling the sample along with the furnace.
FIG. 2 shows K obtained in this example 0.5 Na 0.5 NbO 3 The cross-sectional scanning electron micrograph of the sample can be seen to be K in 1 hour with the aid of an electric field 0.5 Na 0.5 NbO 3 The single crystal grows to about 150 μm.
Meanwhile, the applicant finds that on the basis of adopting a cold isostatic pressing and other pressing forming modes to the single crystal templates with different crystal phases in the step 1, the electric field auxiliary method can also promote the single crystal growth by the solid phase method, and the crystal phases of the single crystal templates can also comprise [111].
Finally, it is noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention.
Claims (10)
1. A method for fast growing single crystal by electric field assisted solid phase method is characterized in that in the process of preparing single crystal by solid phase method, the growth speed of single crystal by solid phase method is accelerated by applying electric field assisted heat treatment.
2. The method for rapid growth of single crystals by electric field assisted solid phase method according to claim 1, comprising the steps of:
step 1: pressing and forming the single crystal template and the target crystal powder together to obtain a ceramic green body;
step 2: pre-sintering the ceramic green body in the step 1;
step 3: and (3) performing heat treatment on the ceramic green body subjected to presintered in the step (2) by adopting an electric field assisted sintering technology, so as to realize the rapid growth of single crystals.
3. The method for rapid growth of single crystals by electric field assisted solid phase method as set forth in claim 2, wherein the single crystal template in step 1 is a single crystal template comprising SrTiO 3 、KTaO 3 Any single crystal template material including [100 ] in crystal phase]、[110]、[111]Any of which is included.
4. The method for rapid growth of single crystals by electric field assisted solid phase method as set forth in claim 2, wherein the target crystal powder in step 1 is SrTiO-containing powder corresponding to a single crystal template 3 、K 0.5 Na 0.5 NbO 3 Any crystal powder.
5. The method for rapid growth of single crystals by electric field assisted solid phase method according to claim 2, wherein the pre-sintering temperature in step 2 is 500-1100 ℃ and the pre-sintering time is 1-24h.
6. The method for rapid growth of single crystals by electric field assisted solid phase method as set forth in claim 2, wherein the electric field assisted sintering technique in step 3 is:
connecting the ceramic green bodies in series into a circuit; then placing the ceramic green body in a heating furnace, heating the ceramic green body to a preset constant temperature, applying a preset constant electric field to the ceramic green body until a flash phenomenon occurs, changing a power supply from a constant voltage state to a constant current state after the flash phenomenon occurs, controlling the current density of the constant current state, keeping for a period of time under the current density, turning off the power supply, turning off the heating furnace, and cooling.
7. The method for rapid growth of single crystals by electric field assisted solid phase method as claimed in claim 6, wherein the electric field assisted sintering technique is further capable of applying a predetermined constant electric field to the green body while heating, and continuously heating until flash sintering occurs.
8. The method for rapid growth of single crystals by electric field assisted solid phase method as set forth in claim 6, wherein the predetermined constant temperature is 600-1100 ℃.
9. The method for rapid growth of single crystals by electric field assisted solid phase method according to any one of claims 6 to 7, wherein the electric field strength of the predetermined constant electric field is 100V/cm to 1000V/cm.
10. The method for rapid growth of single crystals by electric field assisted solid phase method as set forth in claim 6, characterized in that,
the current density of the constant current state is 10mA/mm 2 -1000mA/mm 2 The holding time of the constant current state is 0.5h-240h,
the cooling mode is furnace-following cooling.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310928985.3A CN116905081B (en) | 2023-07-27 | 2023-07-27 | Method for fast growth of single crystal by electric field assisted solid phase method |
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| CN202310928985.3A CN116905081B (en) | 2023-07-27 | 2023-07-27 | Method for fast growth of single crystal by electric field assisted solid phase method |
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| CN116905081A true CN116905081A (en) | 2023-10-20 |
| CN116905081B CN116905081B (en) | 2024-06-25 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172377A (en) * | 2013-04-12 | 2013-06-26 | 常州大学 | Method for preparing high-performance piezoelectric ceramic through reaction solid-phase growth |
| US20150329430A1 (en) * | 2014-05-16 | 2015-11-19 | Applied Materials, Inc. | Advanced layered bulk ceramics via field assisted sintering technology |
| CN110128115A (en) * | 2019-05-23 | 2019-08-16 | 西南交通大学 | A kind of method that flash burning prepares oxide eutectic ceramics |
| CN112919902A (en) * | 2021-03-26 | 2021-06-08 | 上海大学 | Preparation method of electric field assisted low-temperature rapid sintering fine-grain barium titanate capacitor ceramic |
| US20220135489A1 (en) * | 2020-10-29 | 2022-05-05 | Shanghai Jiao Tong University | Method for preparing continuous fiber-reinforced ceramic matrix composite by flash sintering technology |
| CN115159974A (en) * | 2022-06-24 | 2022-10-11 | 东莞理工学院 | SrFeO 3-x Reactive flash firing preparation method of ceramic |
-
2023
- 2023-07-27 CN CN202310928985.3A patent/CN116905081B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172377A (en) * | 2013-04-12 | 2013-06-26 | 常州大学 | Method for preparing high-performance piezoelectric ceramic through reaction solid-phase growth |
| US20150329430A1 (en) * | 2014-05-16 | 2015-11-19 | Applied Materials, Inc. | Advanced layered bulk ceramics via field assisted sintering technology |
| CN110128115A (en) * | 2019-05-23 | 2019-08-16 | 西南交通大学 | A kind of method that flash burning prepares oxide eutectic ceramics |
| US20220135489A1 (en) * | 2020-10-29 | 2022-05-05 | Shanghai Jiao Tong University | Method for preparing continuous fiber-reinforced ceramic matrix composite by flash sintering technology |
| CN112919902A (en) * | 2021-03-26 | 2021-06-08 | 上海大学 | Preparation method of electric field assisted low-temperature rapid sintering fine-grain barium titanate capacitor ceramic |
| CN115159974A (en) * | 2022-06-24 | 2022-10-11 | 东莞理工学院 | SrFeO 3-x Reactive flash firing preparation method of ceramic |
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