CN107268073A - A kind of method that pulling growth prepares LSGM fast-ionic conductor monocrystalline - Google Patents
A kind of method that pulling growth prepares LSGM fast-ionic conductor monocrystalline Download PDFInfo
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- CN107268073A CN107268073A CN201710630881.9A CN201710630881A CN107268073A CN 107268073 A CN107268073 A CN 107268073A CN 201710630881 A CN201710630881 A CN 201710630881A CN 107268073 A CN107268073 A CN 107268073A
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- lsgm
- monocrystalline
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- pulling growth
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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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
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- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A kind of method that pulling growth prepares LSGM fast-ionic conductor monocrystalline, it is possible to resolve the technical problem of the extremely difficult preparation of LSGM monocrystalline of large-size.Comprise the following steps that：Step one：Raw material La2O3, Ga2O3, MgO and SrCO3 are respectively dried standby；Step 2：La2O3 by mass percentage：Ga2O3：SrCO3：MgO=61.1%：35.2%：2.9%：0.8% carries out dispensing；Step 3：Raw material is subjected to briquet after uniform ball mill mixing, pre-fired phase in planetary ball mill, is put into iridium crucible；Step 4：Iridium crucible is put into monocrystal growing furnace, inert gas is passed through, 1,500 1700 DEG C or so are warming up to, using seed rod, it is 1 4mm/h to control pull rate, and seed rod rotary speed is that 10 20rpm carry out pulling growth, and last slow cooling obtains the LSGM monocrystalline of diameter 2 ".The inventive method is simple and convenient, can prepare large-size LSGM monocrystalline, is significant for LSGM monocrystalline and its application study in SOFCs, has effectively filled up the domestic blank in monocrystalline LSGM researchs.
Description
Technical field
The present invention relates to the technical field for preparing LSGM, and in particular to a kind of pulling growth prepares LSGM fast-ionic conductor lists
Brilliant method.
Background technology
LSGM (the La of perovskite structure0.95Sr0.05Ga0.95Mg0.05O3-δ) it is used as solid-oxide fuel cell (SOFCs)
Electrolyte be widely studied, and because it in (600-800 DEG C) of middle warm area has high pure oxygen ion conductance
Rate, can as YSZ favourable replacer.At a lower temperature (700 DEG C of ＜), LSGM ionic conductivity improves 5 compared with YSZ
Times.During typical SOFCs redox reactions, LSGM has high ionic conductivity and negligible electronics electric
Conductance, it is possible to be widely applied as electrolyte.
The method for preparing LSGM at present is mainly high-temperature solid phase reaction method and wet chemical method, using both the above method system
Standby LSGM is polycrystalline structure.Current characterizing method is difficult the shadow for distinguishing crystal grain body and crystal boundary to each chemical property
Ring, in most researchs before, polycrystalline LSGM various performance parameters can not accurately reflect bulk properties, therefore by crystalline substance
Influence and crystal boundary influence to electrical conductivity of the body body to electrical conductivity is made a distinction with very great meaning.Yet with compared with
Large-sized LSGM monocrystalline is extremely difficult to be prepared, therefore up to the present, the domestic research for monocrystalline LSGM is still in blank
State.
The content of the invention
The method that a kind of pulling growth proposed by the present invention prepares LSGM fast-ionic conductor monocrystalline, it is possible to resolve large-size
The technical problem of the extremely difficult preparation of LSGM monocrystalline.
To achieve the above object, present invention employs following technical scheme：
A kind of method that pulling growth prepares LSGM fast-ionic conductor monocrystalline, it is characterised in that：Comprise the following steps that：
Step one：Raw material La2O3, Ga2O3, MgO and SrCO3 are respectively dried standby；
Step 2：La2O3 by mass percentage：Ga2O3：SrCO3：MgO=61.1%：35.2%：2.9%：0.8% enters
Row dispensing；
Step 3：Raw material is subjected to briquet after uniform ball mill mixing, pre-fired phase in planetary ball mill, put
Enter in iridium crucible；
Step 4：Iridium crucible is put into monocrystal growing furnace, inert gas is passed through, 1500-1700 DEG C or so is warming up to, adopted
With seed rod, it is 1-4mm/h to control pull rate, and seed rod rotary speed is that 10-20rpm carries out pulling growth, last slow
Cooling obtains the LSGM monocrystalline of diameter 2 ".
Further, the step one dries raw material La2O3, Ga2O3, MgO at 1000 DEG C, and SrCO3 is at 300 DEG C
Drying.
Further, inert gas is Ar gas in the step 4.
Further, temperature is 1500 DEG C in the step 4, and pull rate is 3mm/h, and rotary speed is 20rpm.
Further, temperature is 1500 DEG C in the step 4, and pull rate is 2mm/h, and rotary speed is 10rpm.
Further, temperature is 1700 DEG C in the step 4, and pull rate is 1mm/h, and rotary speed is 20rpm.
Further, seed crystal uses (001) face LaGaO3 monocrystalline in the step 4.
As shown from the above technical solution, the invention discloses the side that a kind of pulling growth prepares LSGM fast-ionic conductor monocrystalline
Method, by La2O3、Ga2O3、SrCO3And MgO stoichiometrically carries out dispensing, abundant ball milling mixing is uniformly put into iridium earthenware afterwards
Sensing heating melting is carried out in crucible in the range of 1500~1700 DEG C of temperature, while being used as seed using (001) face LaGaO3 monocrystalline
Pulling growth is carried out in the range of crystalline substance, 1~4mm/h of pull rate, seed rod rotary speed 10-20rpm, a diameter of 2 inches are made
LSGM monocrystalline.
The inventive method is simple and convenient, can prepare large-size LSGM monocrystalline, for LSGM monocrystalline and its in SOFCs
In application study be significant, effectively filled up the domestic blank in monocrystalline LSGM researchs.
Embodiment
With reference to embodiment, the present invention will be further described：
Embodiment 1：
A kind of method that pulling growth prepares LSGM fast-ionic conductor monocrystalline, is comprised the following steps that：
(1) raw material prepares and configured
Raw material La2O3, Ga2O3, MgO are dried into 6h at 1000 DEG C, SrCO3 dries 6h at 300 DEG C；
La2O3 by mass percentage：Ga2O3：SrCO3：MgO (wt%)=61.1%：35.2%：2.9%：0.8% enters
Row dispensing；
Raw material is carried out to briquet after the uniform ball mill mixings of 24h, pre-fired phase in planetary ball mill, iridium is put into
In crucible；(2) pulling growth
Iridium crucible is put into monocrystal growing furnace, inert gas is passed through, the present embodiment uses Ar gas, is warming up to 1500 DEG C of left sides
The right side, seed rod is (001) face LaGaO3, and it is 3mm/h to control pull rate, and seed rod rotary speed is that 20rpm carries out lifting life
Long, last slow cooling obtains the LSGM monocrystalline of diameter 2 ".
Embodiment 2：
A kind of method that pulling growth prepares LSGM fast-ionic conductor monocrystalline, is comprised the following steps that：
(1) raw material prepares and configured
Raw material La2O3, Ga2O3, MgO are dried into 6h at 1000 DEG C, SrCO3 dries 6h at 300 DEG C；
La2O3 by mass percentage：Ga2O3：SrCO3：MgO (wt%)=61.1%：35.2%：2.9%：0.8% enters
Row dispensing；
Raw material is carried out to briquet after the uniform ball mill mixings of 24h, pre-fired phase in planetary ball mill, iridium is put into
In crucible；
(2) pulling growth
Iridium crucible is put into monocrystal growing furnace, inert gas is passed through, the present embodiment uses Ar gas, is warming up to 1500 DEG C of left sides
The right side, seed rod is (001) face LaGaO3, and it is 2mm/h to control pull rate, and seed rod rotary speed is that 10rpm carries out lifting life
Long, last slow cooling obtains the LSGM monocrystalline of diameter 2 ".
Embodiment 3：
A kind of method that pulling growth prepares LSGM fast-ionic conductor monocrystalline, is comprised the following steps that：
(1) raw material prepares and configured；
Raw material La2O3, Ga2O3, MgO are dried into 6h at 1000 DEG C, SrCO3 dries 6h at 300 DEG C；
La2O3 by mass percentage：Ga2O3：SrCO3：MgO (wt%)=61.1%：35.2%：2.9%：0.8% enters
Row dispensing；
Raw material is carried out to briquet after the uniform ball mill mixings of 24h, pre-fired phase in planetary ball mill, iridium is put into
In crucible；(2) pulling growth；
Iridium crucible is put into monocrystal growing furnace, inert gas is passed through, the present embodiment uses Ar gas, is warming up to 1700 DEG C of left sides
The right side, seed rod is (001) face LaGaO3, and it is 1mm/h to control pull rate, and seed rod rotary speed is that 20rpm carries out lifting life
Long, last slow cooling obtains the LSGM monocrystalline of diameter 2 ".
The present embodiment simply and easily prepares large-size LSGM monocrystalline in the method for pulling growth, to LSGM bodies
The research of energy is extremely important.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, technical side of the those of ordinary skill in the art to the present invention
Various modifications and improvement that case is made, all should fall within the scope of protection of the present invention.
Claims (7)
1. a kind of method that pulling growth prepares LSGM fast-ionic conductor monocrystalline, it is characterised in that：Comprise the following steps that：
Step one：Raw material La2O3, Ga2O3, MgO and SrCO3 are respectively dried standby；
Step 2：La2O3 by mass percentage：Ga2O3：SrCO3：MgO=61.1%：35.2%：2.9%：0.8% is matched somebody with somebody
Material；
Step 3：Raw material is subjected to briquet after uniform ball mill mixing, pre-fired phase in planetary ball mill, iridium is put into
In crucible；
Step 4：Iridium crucible is put into monocrystal growing furnace, inert gas is passed through, 1500-1700 DEG C or so is warming up to, using seed
Crystalline style, it is 1-4mm/h to control pull rate, and seed rod rotary speed is that 10-20rpm carries out pulling growth, last slow cooling
Obtain the LSGM monocrystalline of diameter 2 ".
2. the method that pulling growth according to claim 1 prepares LSGM fast-ionic conductor monocrystalline, it is characterised in that：It is described
Step one dries raw material La2O3, Ga2O3, MgO at 1000 DEG C, and SrCO3 is dried at 300 DEG C.
3. the method that pulling growth according to claim 2 prepares LSGM fast-ionic conductor monocrystalline, it is characterised in that：It is described
Inert gas is Ar gas in step 4.
4. the method that pulling growth according to claim 3 prepares LSGM fast-ionic conductor monocrystalline, it is characterised in that：It is described
Temperature is 1500 DEG C in step 4, and pull rate is 3mm/h, and rotary speed is 20rpm.
5. the method that pulling growth according to claim 3 prepares LSGM fast-ionic conductor monocrystalline, it is characterised in that：It is described
Temperature is 1500 DEG C in step 4, and pull rate is 2mm/h, and rotary speed is 10rpm.
6. the method that pulling growth according to claim 3 prepares LSGM fast-ionic conductor monocrystalline, it is characterised in that：It is described
Temperature is 1700 DEG C in step 4, and pull rate is 1mm/h, and rotary speed is 20rpm.
7. the method that the pulling growth according to claim 1-6 any one prepares LSGM fast-ionic conductor monocrystalline, it is special
Levy and be：Seed crystal uses (001) face LaGaO3 monocrystalline in the step 4.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710630881.9A CN107268073A (en) | 2017-07-28 | 2017-07-28 | A kind of method that pulling growth prepares LSGM fast-ionic conductor monocrystalline |
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| CN201710630881.9A CN107268073A (en) | 2017-07-28 | 2017-07-28 | A kind of method that pulling growth prepares LSGM fast-ionic conductor monocrystalline |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004117126A (en) * | 2002-09-25 | 2004-04-15 | Tatsuki Ishihara | Hydrocarbon sensor and method for using the same |
| US20080075998A1 (en) * | 2006-09-22 | 2008-03-27 | Tatsumi Ishihara | Electrolyte membrane for electrochemical cell and a method of producing the same |
| CN103715442A (en) * | 2012-09-28 | 2014-04-09 | Toto株式会社 | Solid oxide fuel cell |
-
2017
- 2017-07-28 CN CN201710630881.9A patent/CN107268073A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004117126A (en) * | 2002-09-25 | 2004-04-15 | Tatsuki Ishihara | Hydrocarbon sensor and method for using the same |
| US20080075998A1 (en) * | 2006-09-22 | 2008-03-27 | Tatsumi Ishihara | Electrolyte membrane for electrochemical cell and a method of producing the same |
| CN103715442A (en) * | 2012-09-28 | 2014-04-09 | Toto株式会社 | Solid oxide fuel cell |
Non-Patent Citations (2)
| Title |
|---|
| FENG ZHENG, ET AL.: "Phase constitution in Sr and Mg doped LaGaO3 system", 《MATERIALS RESEARCH BULLETIN》 * |
| M. GLOWACKI, ET AL.: "Growth and characterization of perovskite LaGaO3 crystals doped with Sr and Mn", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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Application publication date: 20171020 |