CN105800654B - A kind of synthetic method for preparing β type Al2O3 solid electrolyte nano-powders - Google Patents
A kind of synthetic method for preparing β type Al2O3 solid electrolyte nano-powders Download PDFInfo
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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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- 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 present invention relates to a kind of synthetic method of nano-powder, particularly one kind to prepare β types Al2O3Mechanico-chemical reaction, the relatively low each serial product of generation energy are occurred for sodium metaaluminate, aluminum oxide, magnesia by the synthetic method of solid electrolyte nano-powder, this method using high-energy ball-milling process.Because the synthetic method is without high-temperature technology, material is obtained as the good nano material of uniformity；Energy consumption is low, does not outwards discharge organic pollution, green；Mechanization degree is high, is adapted to batch production.
Description
Technical field
The present invention relates to a kind of synthetic method of nano-powder, particularly one kind to prepare β types Al2O3Solid electrolyte nanometer
The synthetic method of powder.
Background technology
Solid electrolyte is a kind of mainly solid matter of conduction, also known as fast ion by Ion transfer.It is simultaneously simultaneous
There are solid-state profile and the ionic conductivity of liquid strong electrolyte, be widely used in energy industry, electronics industry, electromechanical integration
Deng field, particularly energy-storage battery and ultracapacitor battery etc..
β types 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 are respectively：β-Al2O3：Na2O•11Al2O3；β’-Al2O3：Na2O•7
Al2O3；β''-Al2O3：Na2O•5.33 Al2O3；β'''-Al2O3：Na2O•4MgO •15Al2O3, β ' ' ' '-Al2O3：
Na1.69Mg2.67Al14.33O25.β types Al2O3β-Al in each series2O3With β ' '-Al2O3Performance is more excellent, belongs to spinel structure.Initially
β-the Al of exploitation2O3, there is very high ionic conductivity at 200-300 DEG C（Up to 0.1S/cm）, can equivalent to the level of fused salt conduction
It is widely used in energy-storage battery material, such as the diaphragm material of Na/S batteries.β"-Al2O3Structure cell is compared to β-Al2O3It is big by 50%,
More one layer of conductive layer, illustrate higher sodium ion conductance（Generally 0.2-0.4S/cm, 300 DEG C）, this is for electrolyte
Using more favourable.
β types Al2O3The current technique of each series mainly have conventional solid-state method（High temperature solid-state method）And liquid phase method（Colloidal sol-solidifying
Glue method, hydrothermal synthesis method, chemical coprecipitation technique etc.）, due to β types Al2O3Each series all needed through too high with above traditional synthesis
Temperature processing（1600 DEG C of high temperature solid-state method, at least more than 1000 DEG C of liquid phase method）, technical process is difficult to control, and nano-powder is more difficult to be obtained
, it is not green to environmental emission organic pollutant during special collosol and gel liquid phase synthesizing method.
The content of the invention
It is an object of the invention to provide a kind of green preparation β types Al2O3The synthesis side of solid electrolyte nano-powder
Method.
The object of the present invention is achieved like this, and one kind prepares β types Al2O3The synthetic method of solid electrolyte nano-powder,
It is characterized in that including at least following steps：
The first step, sodium metaaluminate, aluminum oxide, magnesia are poured into container respectively, container is put into baking oven and dries 6h；
Second step, after drying, three kinds of powders are uniformly mixed by different mol ratio；
3rd step, Ф 20mm and Ф 10mm abrading-ball are added in ball grinder, Ф 20mm and Ф 10mm ratio are 1:2；
4th step, it is 20 by the mass ratio that mixed powder presses ball and powder：1 adds in tank；The cumulative volume of powder and ball
No more than the 2/3 of jar cumulative volume;After discharging material and ball, sealing ring is added on jar, is closed the lid；
5th step, is turned on the power switch, and opens high energy ball mill lid；
6th step, the flow operations tested according to high-energy ball milling, fixes ball grinder and ball milling lid, finally covers enclosing cover lid
Son；
7th step, rotating speed are set： 230rpm；Monocycle technique is set：Ball milling 25 minutes, suspend 5 minutes；Repetition period
Set：47 times；The net Ball-milling Time of technique 20 hours, 24 hours total times；
8th step, machine are started working；
9th step, after 24 hours, open high energy ball mill lid and ball grinder lid takes out synthetic powder；
Tenth step, it is with alcohol washes ball and tank, next time after ball after cleaning and tank drying 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•7 Al2O3；Its raw material ratio is in molar ratio：NaAlO2/
Al2O3/MgO =2/6/0。
Described synthetic powder is β ' '-Al2O3：Na2O•5.33 Al2O3；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 is tungsten-carbide ball material mass fraction containing tungsten carbide 93%, and cobalt 6%, its relative density is 14.75g/
cm3。
Described high energy ball mill is German FRITSCH planetary high-energy ball mills.
It is an advantage of the invention that：It is using high-energy ball-milling process that sodium metaaluminate, aluminum oxide, magnesia generation mechanochemistry is anti-
Should, the relatively low each serial product of generation energy.Because the synthetic method is without high-temperature technology, it is good for uniformity to obtain material
Nano material；Energy consumption is low, does not outwards discharge organic pollution, green；Mechanization degree is high, is adapted to batch production.
Brief description of the drawings
With reference to embodiment and accompanying drawing, the invention will be further described：
Fig. 1 is the XRD of different Ball-milling Time building-up processes.
Embodiment
Embodiment 1
One kind prepares β types Al2O3The synthetic method of solid electrolyte nano-powder, it is characterized in that, including at least following step
Suddenly：
The first step, sodium metaaluminate, aluminum oxide, magnesia are poured into container respectively（Beaker）, container is put into baking oven and dried
Dry 6h；
Second step, after drying, by three kinds of powders in molar ratio：NaAlO2/Al2O3/ MgO=2/6/0 uniformly mixes；
3rd step, Ф 20mm and Ф 10mm abrading-ball are added in ball grinder, Ф 20mm and Ф 10mm ratio are 1:2；
4th step, it is 20 by the mass ratio that mixed powder presses ball and powder：1 adds in tank；The cumulative volume of powder and ball
No more than the 2/3 of jar cumulative volume;After discharging material and ball, sealing ring is added on jar, is closed the lid；
5th step, is turned on the power switch, and opens high energy ball mill lid；
6th step, the flow operations tested according to high-energy ball milling, fixes ball grinder and ball milling lid, finally covers enclosing cover lid
Son；
7th step, rotating speed are set： 230rpm；Monocycle technique is set：Ball milling 25 minutes, suspend 5 minutes；Repetition period
Set：47 times；The net Ball-milling Time of technique 20 hours, 24 hours total times；
8th step, machine are started working；
9th step, after 24 hours, open high energy ball mill lid and ball grinder lid takes out the β-Al of synthesis2O3：Na2O•
11Al2O3Powder；
Tenth step, it is with alcohol washes ball and tank, next time after ball after cleaning and tank drying is standby.
Embodiment 2
One kind prepares β types Al2O3The synthetic method of solid electrolyte nano-powder, it is characterized in that, including at least following step
Suddenly：
The first step, sodium metaaluminate, aluminum oxide, magnesia are poured into container respectively（Beaker）, container is put into baking oven and dried
Dry 6h；
Second step, after drying, by three kinds of powders in molar ratio：NaAlO2/Al2O3/MgO =2/6/0；
3rd step, Ф 20mm and Ф 10mm abrading-ball are added in ball grinder, Ф 20mm and Ф 10mm ratio are 1:2；
4th step, it is 20 by the mass ratio that mixed powder presses ball and powder：1 adds in tank；The cumulative volume of powder and ball
No more than the 2/3 of jar cumulative volume;After discharging material and ball, sealing ring is added on jar, is closed the lid；
5th step, is turned on the power switch, and opens high energy ball mill lid；
6th step, the flow operations tested according to high-energy ball milling, fixes ball grinder and ball milling lid, finally covers enclosing cover lid
Son；
7th step, rotating speed are set： 230rpm；Monocycle technique is set：Ball milling 25 minutes, suspend 5 minutes；Repetition period
Set：47 times；The net Ball-milling Time of technique 20 hours, 24 hours total times；
8th step, machine are started working；
9th step, after 24 hours, open high energy ball mill lid and ball grinder lid takes out β ' the '-Al of synthesis2O3：
Na2O•5.33 Al2O；
Tenth step, it is with alcohol washes ball and tank, next time after ball after cleaning and tank drying is standby.
Embodiment 3
One kind prepares β types Al2O3The synthetic method of solid electrolyte nano-powder, it is characterized in that, including at least following step
Suddenly：
The first step, sodium metaaluminate, aluminum oxide, magnesia are poured into container respectively（Beaker）, container is put into baking oven and dried
Dry 6h；
Second step, after drying, by three kinds of powders in molar ratio：NaAlO2/Al2O3/MgO =2/4.33/0；
3rd step, Ф 20mm and Ф 10mm abrading-ball are added in ball grinder, Ф 20mm and Ф 10mm ratio are 1:2；
4th step, it is 20 by the mass ratio that mixed powder presses ball and powder：1 adds in tank；The cumulative volume of powder and ball
No more than the 2/3 of jar cumulative volume;After discharging material and ball, sealing ring is added on jar, is closed the lid；
5th step, is turned on the power switch, and opens high energy ball mill lid；
6th step, the flow operations tested according to high-energy ball milling, fixes ball grinder and ball milling lid, finally covers enclosing cover lid
Son；
7th step, rotating speed are set： 230rpm；Monocycle technique is set：Ball milling 25 minutes, suspend 5 minutes；Repetition period
Set：47 times；The net Ball-milling Time of technique 20 hours, 24 hours total times；
8th step, machine are started working；
9th step, after 24 hours, open high energy ball mill lid and ball grinder lid takes out β ' the '-Al of synthesis2O3：
Na2O•5.33 Al2O3；
Tenth step, it is with alcohol washes ball and tank, next time after ball after cleaning and tank drying is standby.
Embodiment 4
One kind prepares β types Al2O3The synthetic method of solid electrolyte nano-powder, it is characterized in that, including at least following step
Suddenly：
The first step, sodium metaaluminate, aluminum oxide, magnesia are poured into container respectively（Beaker）, container is put into baking oven and dried
Dry 6h；
Second step, after drying, by three kinds of powders in molar ratio：NaAlO2/Al2O3/MgO=2/14/4；
3rd step, Ф 20mm and Ф 10mm abrading-ball are added in ball grinder, Ф 20mm and Ф 10mm ratio are 1:2；
4th step, it is 20 by the mass ratio that mixed powder presses ball and powder：1 adds in tank；The cumulative volume of powder and ball
No more than the 2/3 of jar cumulative volume;After discharging material and ball, sealing ring is added on jar, is closed the lid；
5th step, is turned on the power switch, and opens high energy ball mill lid；
6th step, the flow operations tested according to high-energy ball milling, fixes ball grinder and ball milling lid, finally covers enclosing cover lid
Son；
7th step, rotating speed are set： 230rpm；Monocycle technique is set：Ball milling 25 minutes, suspend 5 minutes；Repetition period
Set：47 times；The net Ball-milling Time of technique 20 hours, 24 hours total times；
8th step, machine are started working；
9th step, after 24 hours, open high energy ball mill lid and ball grinder lid takes out β ' ' the '-Al of synthesis2O3：
Na2O•4MgO •15Al2O3；
Tenth step, it is with alcohol washes ball and tank, next time after ball after cleaning and tank drying is standby.
Embodiment 5
One kind prepares β types Al2O3The synthetic method of solid electrolyte nano-powder, it is characterized in that, including at least following step
Suddenly：
The first step, sodium metaaluminate, aluminum oxide, magnesia are poured into container respectively（Beaker）, container is put into baking oven and dried
Dry 6h；
Second step, after drying, by three kinds of powders in molar ratio：NaAlO2/Al2O3/MgO=1.69/6.32/2.67；
3rd step, Ф 20mm and Ф 10mm abrading-ball are added in ball grinder, Ф 20mm and Ф 10mm ratio are 1:2；
4th step, it is 20 by the mass ratio that mixed powder presses ball and powder：1 adds in tank；The cumulative volume of powder and ball
No more than the 2/3 of jar cumulative volume;After discharging material and ball, sealing ring is added on jar, is closed the lid；
5th step, is turned on the power switch, and opens high energy ball mill lid；
6th step, the flow operations tested according to high-energy ball milling, fixes ball grinder and ball milling lid, finally covers enclosing cover lid
Son；
7th step, rotating speed are set： 230rpm；Monocycle technique is set：Ball milling 25 minutes, suspend 5 minutes；Repetition period
Set：47 times；The net Ball-milling Time of technique 20 hours, 24 hours total times；
8th step, machine are started working；
9th step, after 24 hours, open high energy ball mill lid and ball grinder lid takes out β ' ' ' the '-Al of synthesis2O3：
Na1.69Mg2.67Al14.33O25；
Tenth step, it is with alcohol washes ball and tank, next time after ball after cleaning and tank drying is standby.
In the present invention in each implementation process, high-energy ball milling hour time is different, and average grain size therein is different
, shown in Fig. 1 XRD results, by the net High Energy Ball Milling Time of 20 hours, crystalline phase needed for synthesis, calculated through Scherrer formula
Average grain size is 30nm or so.
High energy ball mill used in the present invention is German FRITSCH planetary high-energy ball mills.Tungsten-carbide ball grinding jar
（Single tank；Double tanks；Four tanks are optional, supporting with ball mill）；Tungsten-carbide ball Ф 20mm and Ф 10mm ball.Tungsten carbide material（It is carbon containing
Change tungsten mass fraction 93%, cobalt 6%）, its relative density is 14.75g/cm3。
Claims (2)
1. one kind prepares β types Al2O3The synthetic method of solid electrolyte nano-powder, it is characterized in that, including at least following steps：
The first step, sodium metaaluminate, aluminum oxide, magnesia are poured into container respectively, container is put into baking oven and dries 6h；
Second step, after drying, three kinds of powders are uniformly mixed by different mol ratio；
3rd step, Ф 20mm and Ф 10mm abrading-ball are added in ball grinder, Ф 20mm and Ф 10mm ratio are 1:2；
4th step, it is 20 by the mass ratio that mixed powder presses ball and powder：1 adds in tank；The cumulative volume of powder and ball does not surpass
Cross the 2/3 of jar cumulative volume；After discharging material and ball, sealing ring is added on jar, is closed the lid；
5th step, is turned on the power switch, and opens high energy ball mill lid；
6th step, the flow operations tested according to high-energy ball milling, fixes ball grinder and ball milling lid, finally covers enclosing cover lid；
7th step, rotating speed are set：230rpm；Monocycle technique is set：Ball milling 25 minutes, suspend 5 minutes；Repetition period is set：
47 times；The net Ball-milling Time of technique 20 hours, 24 hours total times；
8th step, machine are started working；
9th step, after 24 hours, open high energy ball mill lid and ball grinder lid takes out synthetic powder；
Tenth step, it is with alcohol washes ball and tank, next time after ball after cleaning and tank drying is standby；
Described synthetic powder is β-Al2O3：Na2O·11Al2O3, its raw material ratio is in molar ratio：NaAlO2/Al2O3/
MgO=2/10/0；Or described synthetic powder is β '-Al2O3：Na2O·7Al2O3, its raw material ratio is in molar ratio：
NaAlO2/Al2O3/ MgO=2/6/0；Or described synthetic powder is β "-Al2O3：Na2O·5.33Al2O3, its raw material ratio
It is in molar ratio：NaAlO2/Al2O3/ MgO=2/4.33/0；Or described synthetic powder is β " '-Al2O3：Na2O·4MgO·
15Al2O3, its raw material ratio is in molar ratio：NaAlO2/Al2O3/ MgO=2/14/4；Or 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 is tungsten-carbide ball material mass fraction containing tungsten carbide 93%, and cobalt 6%, its relative density is 14.75g/
cm3。
2. one kind according to claim 1 prepares β types Al2O3The synthetic method of solid electrolyte nano-powder, its feature
It is：High energy ball mill is German FRITSCH planetary high-energy ball mills.
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| CN104276816B (en) * | 2013-07-12 | 2016-08-10 | 中国科学院上海硅酸盐研究所 | The method of sode cell electrolyte membrance is prepared in sprayed deposit molding |
| CN105152634B (en) * | 2015-08-09 | 2017-06-20 | 宁夏绿聚能电源有限公司 | Sodium nickel-based battery electrolyte β " Al2O3The preparation method of ceramics |
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