CN105800654A - Synthesis method for preparing beta-type Al2O3 solid electrolyte nano powder - Google Patents
Synthesis method for preparing beta-type Al2O3 solid electrolyte nano powder Download PDFInfo
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- CN105800654A CN105800654A CN201610130780.0A CN201610130780A CN105800654A CN 105800654 A CN105800654 A CN 105800654A CN 201610130780 A CN201610130780 A CN 201610130780A CN 105800654 A CN105800654 A CN 105800654A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention relates to a synthesis method for nano powder, in particular to a synthesis method for preparing beta-type Al2O3 solid electrolyte nano powder, According to the synthesis method, a high energy ball milling technique is adopted to enable sodium metaaluminate, aluminum oxide and magnesium oxide to have mechanical chemical reaction, and then series of products with relatively low energy can be generated. The synthesis method has no high-temperature process, the material produced by using the synthesis method is a nano material with good uniformity, the energy consumption is low, no organic pollutant can be discharged out, and the synthesis method is environmentally friendly, high in mechanical degree and applicable to large-scale production.
Description
Technical field
The present invention relates to the synthetic method of a kind of nano-powder, particularly one and prepare β type Al2O3The synthetic method of solid electrolyte nano-powder.
Background technology
Solid electrolyte is a kind of solid matter mainly conducted electricity by ion migration, is also called fast ion.It has solid-state profile and the ionic conductivity of liquid strong electrolyte concurrently simultaneously, is widely used in the fields such as energy industry, electronics industry, electromechanical integration, particularly energy-storage battery and ultracapacitor battery etc..
β type Al2O3There is following series, belong to nA2O3-M2O(A3+=Al3+,Ga3+,Fe3+, M+=Na+,K+,Rb+,Ag+,Tl+,H3O+) non-stoichiometric compound, its each series is respectively as follows: β-Al2O3: Na2O·11Al2O3；β’-Al2O3: Na2O·7Al2O3；β''-Al2O3: Na2O·5.33Al2O3；β'''-Al2O3: Na2O·4MgO·15Al2O3, β ' ' ' '-Al2O3: Na1.69Mg2.67Al14.33O25.β type Al2O3β-Al in each series2O3With β ' '-Al2O3Performance is more excellent, belongs to spinel structure.β-the Al being originally developed2O3, have significantly high ionic conductivity (reaching 0.1S/cm) at 200-300 DEG C, be equivalent to the level of fused salt conduction, can be widely used in energy-storage battery material, such as the diaphragm material of Na/S battery.β"-Al2O3Structure cell is compared to β-Al2O3Big 50%, many one layer of conductive layers, illustrate higher sodium ion conductivity (being generally 0.2-0.4S/cm, 300 DEG C), this is more favourable for electrolytical application.
β type Al2O3The current technique of each series mainly have conventional solid-state method (high temperature solid-state method) and liquid phase method (sol-gel process, hydrothermal synthesis method, chemical coprecipitation technique etc.), due to β type Al2O3Each series all need through high-temperature process (high temperature solid-state method 1600 DEG C by above traditional synthesis, liquid phase method more than at least 1000 DEG C), technical process is difficult to control to, the more difficult acquisition of nano-powder, to environmental emission organic pollutant, not environmental protection in special collosol and gel liquid phase synthesizing method process.
Summary of the invention
It is an object of the invention to provide the preparation β type Al of a kind of environmental protection2O3The synthetic method of solid electrolyte nano-powder.
The object of the present invention is achieved like this, and one prepares β type Al2O3The synthetic method of solid electrolyte nano-powder, is characterized in that, at least comprises the steps:
The first step, pours sodium metaaluminate, aluminium oxide, magnesium oxide into container respectively, and container is put into drying 6h in baking oven；
Second step, after drying, by three kinds of powder body by different mol ratio Homogeneous phase mixing；
3rd step, adds the abrading-ball of Ф 20mm and Ф 10mm in ball grinder, and the ratio of Ф 20mm and Ф 10mm is 1:2；
4th step, is that 20:1 adds in tank by mixed powder body by the mass ratio of ball Yu powder；The cumulative volume of powder body and ball is less than the 2/3 of jar cumulative volume;After discharging material and ball, plus sealing ring on jar, cover lid；
5th step, turns on the power switch, and opens high energy ball mill lid；
6th step, according to the flow operations of high-energy ball milling experiment, fixes ball grinder and ball milling lid, finally builds enclosing cover lid；
7th step, rotating speed is arranged: 230rpm；Monocycle technique is arranged: ball milling 25 minutes, suspends 5 minutes；Repetition period is arranged: 47 times；The clean Ball-milling Time of technique 20 hours, 24 hours total times；
8th step, machine is started working；
9th step, after 24 hours, opens high energy ball mill lid and ball grinder lid takes out synthetic powder；
Tenth step, with alcohol washes ball and tank, after after cleaning, ball and tank are dried, next time is standby.
Described synthetic powder is β-Al2O3: Na2O·11Al2O3；Its raw material ratio is in molar ratio: NaAlO2/Al2O3/MgO=2/10/0。
Described synthetic powder is β '-Al2O3: Na2O·7Al2O3；Its raw material ratio is in molar ratio: NaAlO2/Al2O3/MgO=2/6/0。
Described synthetic powder is β ' '-Al2O3: Na2O·5.33Al2O3；Its raw material ratio is in molar ratio: NaAlO2/Al2O3/MgO=2/4.33/0。
Described synthetic powder is β ' ' '-Al2O3: Na2O·4MgO·15Al2O3；Its raw material ratio is in molar ratio: NaAlO2/Al2O3/MgO=2/14/4。
Described synthetic powder is β ' ' ' '-Al2O3: Na1.69Mg2.67Al14.33O25；Its raw material ratio is in molar ratio: NaAlO2/Al2O3/MgO=1.69/6.32/2.67。
Described abrading-ball be tungsten-carbide ball material containing tungsten carbide mass fraction 93%, cobalt 6%, its relative density is 14.75g/cm3。
Described high energy ball mill is Germany's FRITSCH planetary high-energy ball mill.
The invention have the advantage that and utilize high-energy ball-milling process by sodium metaaluminate, aluminium oxide, magnesium oxide generation mechanico-chemical reaction, generate each series product that energy is relatively low.Owing to this synthetic method is without high-temperature technology, obtained material is the nano material that uniformity is good；Energy consumption is low, does not outwards discharge organic pollution, environmental protection；Mechanization degree is high, is suitable for batch production.
Accompanying drawing explanation
Below in conjunction with embodiment and accompanying drawing, the invention will be further described:
Fig. 1 is the XRD figure of different Ball-milling Time building-up process.
Detailed description of the invention
Embodiment 1
One prepares β type Al2O3The synthetic method of solid electrolyte nano-powder, is characterized in that, at least comprises the steps:
The first step, pours container (beaker) respectively into by sodium metaaluminate, aluminium oxide, magnesium oxide, and container is put into drying 6h in baking oven；
Second step, after drying, by three kinds of powder body in molar ratio: NaAlO2/Al2O3/ MgO=2/6/0 Homogeneous phase mixing；
3rd step, adds the abrading-ball of Ф 20mm and Ф 10mm in ball grinder, and the ratio of Ф 20mm and Ф 10mm is 1:2；
4th step, is that 20:1 adds in tank by mixed powder body by the mass ratio of ball Yu powder；The cumulative volume of powder body and ball is less than the 2/3 of jar cumulative volume;After discharging material and ball, plus sealing ring on jar, cover lid；
5th step, turns on the power switch, and opens high energy ball mill lid；
6th step, according to the flow operations of high-energy ball milling experiment, fixes ball grinder and ball milling lid, finally builds enclosing cover lid；
7th step, rotating speed is arranged: 230rpm；Monocycle technique is arranged: ball milling 25 minutes, suspends 5 minutes；Repetition period is arranged: 47 times；The clean Ball-milling Time of technique 20 hours, 24 hours total times；
8th step, machine is started working；
9th step, after 24 hours, opens high energy ball mill lid and ball grinder lid takes out the β-Al synthesized2O3: Na2O·11Al2O3Powder body；
Tenth step, with alcohol washes ball and tank, after after cleaning, ball and tank are dried, next time is standby.
Embodiment 2
One prepares β type Al2O3The synthetic method of solid electrolyte nano-powder, is characterized in that, at least comprises the steps:
The first step, pours container (beaker) respectively into by sodium metaaluminate, aluminium oxide, magnesium oxide, and container is put into drying 6h in baking oven；
Second step, after drying, by three kinds of powder body in molar ratio: NaAlO2/Al2O3/MgO=2/6/0；
3rd step, adds the abrading-ball of Ф 20mm and Ф 10mm in ball grinder, and the ratio of Ф 20mm and Ф 10mm is 1:2；
4th step, is that 20:1 adds in tank by mixed powder body by the mass ratio of ball Yu powder；The cumulative volume of powder body and ball is less than the 2/3 of jar cumulative volume;After discharging material and ball, plus sealing ring on jar, cover lid；
5th step, turns on the power switch, and opens high energy ball mill lid；
6th step, according to the flow operations of high-energy ball milling experiment, fixes ball grinder and ball milling lid, finally builds enclosing cover lid；
7th step, rotating speed is arranged: 230rpm；Monocycle technique is arranged: ball milling 25 minutes, suspends 5 minutes；Repetition period is arranged: 47 times；The clean Ball-milling Time of technique 20 hours, 24 hours total times；
8th step, machine is started working；
9th step, after 24 hours, opens high energy ball mill lid and ball grinder lid takes out β ' the '-Al synthesized2O3: Na2O·5.33Al2O；
Tenth step, with alcohol washes ball and tank, after after cleaning, ball and tank are dried, next time is standby.
Embodiment 3
One prepares β type Al2O3The synthetic method of solid electrolyte nano-powder, is characterized in that, at least comprises the steps:
The first step, pours container (beaker) respectively into by sodium metaaluminate, aluminium oxide, magnesium oxide, and container is put into drying 6h in baking oven；
Second step, after drying, by three kinds of powder body in molar ratio: NaAlO2/Al2O3/MgO=2/4.33/0；
3rd step, adds the abrading-ball of Ф 20mm and Ф 10mm in ball grinder, and the ratio of Ф 20mm and Ф 10mm is 1:2；
4th step, is that 20:1 adds in tank by mixed powder body by the mass ratio of ball Yu powder；The cumulative volume of powder body and ball is less than the 2/3 of jar cumulative volume;After discharging material and ball, plus sealing ring on jar, cover lid；
5th step, turns on the power switch, and opens high energy ball mill lid；
6th step, according to the flow operations of high-energy ball milling experiment, fixes ball grinder and ball milling lid, finally builds enclosing cover lid；
7th step, rotating speed is arranged: 230rpm；Monocycle technique is arranged: ball milling 25 minutes, suspends 5 minutes；Repetition period is arranged: 47 times；The clean Ball-milling Time of technique 20 hours, 24 hours total times；
8th step, machine is started working；
9th step, after 24 hours, opens high energy ball mill lid and ball grinder lid takes out β ' the '-Al synthesized2O3: Na2O·5.33Al2O3；
Tenth step, with alcohol washes ball and tank, after after cleaning, ball and tank are dried, next time is standby.
Embodiment 4
One prepares β type Al2O3The synthetic method of solid electrolyte nano-powder, is characterized in that, at least comprises the steps:
The first step, pours container (beaker) respectively into by sodium metaaluminate, aluminium oxide, magnesium oxide, and container is put into drying 6h in baking oven；
Second step, after drying, by three kinds of powder body in molar ratio: NaAlO2/Al2O3/MgO=2/14/4；
3rd step, adds the abrading-ball of Ф 20mm and Ф 10mm in ball grinder, and the ratio of Ф 20mm and Ф 10mm is 1:2；
4th step, is that 20:1 adds in tank by mixed powder body by the mass ratio of ball Yu powder；The cumulative volume of powder body and ball is less than the 2/3 of jar cumulative volume;After discharging material and ball, plus sealing ring on jar, cover lid；
5th step, turns on the power switch, and opens high energy ball mill lid；
6th step, according to the flow operations of high-energy ball milling experiment, fixes ball grinder and ball milling lid, finally builds enclosing cover lid；
7th step, rotating speed is arranged: 230rpm；Monocycle technique is arranged: ball milling 25 minutes, suspends 5 minutes；Repetition period is arranged: 47 times；The clean Ball-milling Time of technique 20 hours, 24 hours total times；
8th step, machine is started working；
9th step, after 24 hours, opens high energy ball mill lid and ball grinder lid takes out β ' ' the '-Al synthesized2O3: Na2O·4MgO·15Al2O3；
Tenth step, with alcohol washes ball and tank, after after cleaning, ball and tank are dried, next time is standby.
Embodiment 5
One prepares β type Al2O3The synthetic method of solid electrolyte nano-powder, is characterized in that, at least comprises the steps:
The first step, pours container (beaker) respectively into by sodium metaaluminate, aluminium oxide, magnesium oxide, and container is put into drying 6h in baking oven；
Second step, after drying, by three kinds of powder body in molar ratio: NaAlO2/Al2O3/MgO=1.69/6.32/2.67；
3rd step, adds the abrading-ball of Ф 20mm and Ф 10mm in ball grinder, and the ratio of Ф 20mm and Ф 10mm is 1:2；
4th step, is that 20:1 adds in tank by mixed powder body by the mass ratio of ball Yu powder；The cumulative volume of powder body and ball is less than the 2/3 of jar cumulative volume;After discharging material and ball, plus sealing ring on jar, cover lid；
5th step, turns on the power switch, and opens high energy ball mill lid；
6th step, according to the flow operations of high-energy ball milling experiment, fixes ball grinder and ball milling lid, finally builds enclosing cover lid；
7th step, rotating speed is arranged: 230rpm；Monocycle technique is arranged: ball milling 25 minutes, suspends 5 minutes；Repetition period is arranged: 47 times；The clean Ball-milling Time of technique 20 hours, 24 hours total times；
8th step, machine is started working；
9th step, after 24 hours, opens high energy ball mill lid and ball grinder lid takes out β ' ' ' the '-Al synthesized2O3: Na1.69Mg2.67Al14.33O25；
Tenth step, with alcohol washes ball and tank, after after cleaning, ball and tank are dried, next time is standby.
In the present invention in each implementation process, time high-energy ball milling hour is different, and average grain size therein is different, shown in Fig. 1 XRD result, through the clean High Energy Ball Milling Time of 20 hours, the required crystalline phase of synthesis, calculating average grain size through Scherrer formula was about 30nm.
High energy ball mill used in the present invention is Germany's FRITSCH planetary high-energy ball mill.Tungsten-carbide ball grinding jar (single tank；Double; two tanks；Four tanks are optional, supporting with ball mill)；The ball of tungsten-carbide ball Ф 20mm and Ф 10mm.Tungsten carbide material (containing tungsten carbide mass fraction 93%, cobalt 6%), its relative density is 14.75g/cm3。
Claims (8)
1. prepare β type Al for one kind2O3The synthetic method of solid electrolyte nano-powder, is characterized in that, at least comprises the steps:
The first step, pours sodium metaaluminate, aluminium oxide, magnesium oxide into container respectively, and container is put into drying 6h in baking oven；
Second step, after drying, by three kinds of powder body by different mol ratio Homogeneous phase mixing；
3rd step, adds the abrading-ball of Ф 20mm and Ф 10mm in ball grinder, and the ratio of Ф 20mm and Ф 10mm is 1:2；
4th step, is that 20:1 adds in tank by mixed powder body by the mass ratio of ball Yu powder；The cumulative volume of powder body and ball is less than the 2/3 of jar cumulative volume;After discharging material and ball, plus sealing ring on jar, cover lid；
5th step, turns on the power switch, and opens high energy ball mill lid；
6th step, according to the flow operations of high-energy ball milling experiment, fixes ball grinder and ball milling lid, finally builds enclosing cover lid；
7th step, rotating speed is arranged: 230rpm；Monocycle technique is arranged: ball milling 25 minutes, suspends 5 minutes；Repetition period is arranged: 47 times；The clean Ball-milling Time of technique 20 hours, 24 hours total times；
8th step, machine is started working；
9th step, after 24 hours, opens high energy ball mill lid and ball grinder lid takes out synthetic powder；
Tenth step, with alcohol washes ball and tank, after after cleaning, ball and tank are dried, next time is standby.
2. one according to claim 1 prepares β type Al2O3The synthetic method of solid electrolyte nano-powder, is characterized in that: described synthetic powder is β-Al2O3: Na2O·11Al2O3；Its raw material ratio is in molar ratio: NaAlO2/Al2O3/MgO=2/10/0。
3. one according to claim 1 prepares β type Al2O3The synthetic method of solid electrolyte nano-powder, is characterized in that: described synthetic powder is β '-Al2O3: Na2O·7Al2O3；Its raw material ratio is in molar ratio: NaAlO2/Al2O3/MgO=2/6/0。
4. one according to claim 1 prepares β type Al2O3The synthetic method of solid electrolyte nano-powder, is characterized in that: described synthetic powder is β ' '-Al2O3: Na2O·5.33Al2O3；Its raw material ratio is in molar ratio: NaAlO2/Al2O3/MgO=2/4.33/0。
5. one according to claim 1 prepares β type Al2O3The synthetic method of solid electrolyte nano-powder, is characterized in that: described synthetic powder is β ' ' '-Al2O3: Na2O·4MgO·15Al2O3；Its raw material ratio is in molar ratio: NaAlO2/Al2O3/MgO=2/14/4。
6. one according to claim 1 prepares β type Al2O3The synthetic method of solid electrolyte nano-powder, is characterized in that: described synthetic powder is β ' ' ' '-Al2O3: Na1.69Mg2.67Al14.33O25；Its raw material ratio is in molar ratio: NaAlO2/Al2O3/MgO=1.69/6.32/2.67。
7. one according to claim 1 prepares β type Al2O3The synthetic method of solid electrolyte nano-powder, is characterized in that: described abrading-ball be tungsten-carbide ball material containing tungsten carbide mass fraction 93%, cobalt 6%, its relative density is 14.75g/cm3。
8. one according to claim 1 prepares β type Al2O3The synthetic method of solid electrolyte nano-powder, is characterized in that: described high energy ball mill is Germany's FRITSCH planetary high-energy ball mill.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86104187A (en) * | 1985-05-24 | 1987-04-29 | 利利怀特公司 | β " the preparation method of aluminum oxide |
| CN104276816A (en) * | 2013-07-12 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | Method for preparing sodium battery electrolyte membrane by employing spray deposition molding |
| CN105152634A (en) * | 2015-08-09 | 2015-12-16 | 宁夏绿聚能电源有限公司 | Preparation method of beta''-Al2O3 ceramic for Na-Ni battery electrolyte |
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2016
- 2016-03-09 CN CN201610130780.0A patent/CN105800654B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86104187A (en) * | 1985-05-24 | 1987-04-29 | 利利怀特公司 | β " the preparation method of aluminum oxide |
| CN104276816A (en) * | 2013-07-12 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | Method for preparing sodium battery electrolyte membrane by employing spray deposition molding |
| CN105152634A (en) * | 2015-08-09 | 2015-12-16 | 宁夏绿聚能电源有限公司 | Preparation method of beta''-Al2O3 ceramic for Na-Ni battery electrolyte |
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