CN104098118A - Preparation method for high-ion-flux beta''-Al2O3 precusor powder - Google Patents
Preparation method for high-ion-flux beta''-Al2O3 precusor powder Download PDFInfo
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- CN104098118A CN104098118A CN201310128275.9A CN201310128275A CN104098118A CN 104098118 A CN104098118 A CN 104098118A CN 201310128275 A CN201310128275 A CN 201310128275A CN 104098118 A CN104098118 A CN 104098118A
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- China
- Prior art keywords
- boehmite
- pseudo
- preparation
- sodium salt
- precursor powder
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Abstract
A preparation method for a high-ion-flux beta''-Al2O3 precusor powder is characterized by comprising employing pseudo-boehmite as an aluminium source, taking HNO3 as a peptizing agent, so as to obtain a stalbe pseudo-boehmite colloid; dissolving a sodium salt in a solvent to ionizing into Na<+>, then mixing the sodium salt solution with the pseudo-boehmite colloid, so as to enable Na<+> to be adsorbed to pseudo-boehmite particles under the electrostatic attraction effect, and further to obtain a stable composite colloid; and employing a spraying dryer to dry the colloid to obtain a xerogel; and finally performing heat processing at a certain temperature, so as to obtain the beta''-Al2O3 precusor powder.
Description
Technical field
A kind of β 〞-Al of high ion flux
2o
3the preparation method of precursor powder, belongs to chemical field.
Background technology
β 〞-Al
2o
3pottery, owing to having higher sodium ion-conductive, is used as the solid electrolyte material of sodium-sulfur cell, and the quality of its quality will affect performance and the life-span of battery to a great extent.β 〞-Al
2o
3pottery requires to have high sodium ion-conductive, high-compactness and higher physical strength as solid electrolyte, also needs in addition to have uniform microstructure and composition profiles.
β 〞-Al
2o
3the preparation of pottery is mainly divided into three steps: β 〞-Al
2o
3the preparation of precursor powder; β 〞-Al
2o
3ceramic green moulding; By green sintering finished product.β 〞-Al wherein
2o
3the quality of precursor powder quality directly affects the performance of final ceramic objects.Precursor powder is that material powder obtains through roughing, preparation β 〞-Al
2o
3the traditional method of precursor powder is solid reaction process.Solid reaction process adopts the compound that contains aluminium, sodium (as α-Al
2o
3, Na
2cO
3or Na
2c
2o
4) be raw material, add a small amount of Li
2o or MgO, as stablizer, mix through long-time ball milling, and thermal treatment temp is about 1200 ℃, and sintering processes temperature is more than 1600 ℃.Solid reaction process technique is simple, and production cost is low, and facility investment is little, but mixing of materials is inhomogeneous, and this can cause ceramic crystalline phase not single, conductivity variation, and also high-temperature heat treatment can cause Na for a long time
2a large amount of volatilizations of O, this just means the decline of ionic conductivity.
Summary of the invention
The present invention is just in order to solve β 〞-Al
2o
3in powder preparation process, the inhomogeneous and Na of mixing of materials runs off the technical problem such as serious and a kind of β 〞-Al of high ion flux is provided
2o
3the preparation method of precursor powder.
Technical scheme of the present invention is: adopt pseudo-boehmite as the source of aluminium, HNO
3as peptizing agent, can obtain stable Pseudo-boehmite.Sodium salt is dissolved in solvent, makes its ion turn to Na
+, then sodium salt solution is mixed mutually to Na with Pseudo-boehmite
+under electrostatic attraction effect, be adsorbed on pseudo-boehmite particle, obtain stable composite gel, adopt the dry colloidal sol of spray-dryer to obtain xerogel, finally thermal treatment at a certain temperature, obtains β 〞-Al
2o
3precursor powder.
β 〞-the Al of a kind of high ion flux the present invention relates to
2o
3the preparation method of precursor powder, comprises the following steps:
Step 1, appropriate sodium salt is dissolved in a certain amount of solvent, vigorous stirring until dissolve completely, is made into sodium salt solution.
Step 2, appropriate pseudo-boehmite powder is mixed with certain proportion with deionized water, ultrasonic dispersion 30min drips the dilute nitric acid solution of 5mol/L under intense mechanical stirs, and regulating PH is 2 ~ 4, continues to stir 3h, obtains the colloid of stable transparent.
Step 3, sodium salt solution is mixed with Pseudo-boehmite, stir.
Colloidal sol in step 4, employing spray-dryer drying step 3 obtains xerogel.
Step 5, by the xerogel obtaining in step 4 thermal treatment 2 ~ 10h at 500 ℃ ~ 900 ℃, remove organism.
Step 6, with ethanol, as medium, the material that obtains of step 5 is carried out to ball milling 5 ~ 20h, obtain β 〞-Al
2o
3precursor powder.
Further, the sodium salt in step 1 is NaNO
3, NaCOOCH
3, Na
2c
2o
4or Na
2sO
4, solvent for use is preferably deionized water, and solvent adding amount should be able to dissolve above-mentioned sodium salt completely.
Further, in step 3, keeping in pseudo-boehmite mole proportioning of Na element in Al element and sodium salt is 4:1 ~ 11:1.
Further, in step 4, thermal treatment temp is 600 ℃ ~ 900 ℃.
The chemical formula of pseudo-boehmite of the present invention is A1OOHnH
2o(0<n<1), be that water content is greater than boehmite and size of microcrystal is less than the aluminum oxide of boehmite.Pseudo-boehmite can experience by γ-AlOOH → γ-Al in the process heating up
2o
3→ δ-Al
2o
3→ θ-Al
2o
3→ α-Al
2o
3transformation.Acid Dispersion Property of Pseudoboehmite is better, and metal ion is had to very strong adsorptive power, and the uniform and stable composite gel of microscale of formation is conducive to the better β 〞-Al of processability
2o
3material.
The invention has the beneficial effects as follows, select pseudo-boehmite as the source of aluminium, utilize the method for colloidal sol to strengthen the stability of slurries and the homogeneity of mixing of materials.The more important thing is, because pseudo-boehmite granularity is superfine, reach or approach colloidal solid granularity, these fine particles can become glue core, and the double electrical layers forming in its surface, by Na
+be adsorbed on securely solid surface.When colloid is heat-treated, pseudo-boehmite undergoes phase transition into γ-Al from amorphous state
2o
3, in the process of phase transformation, be adsorbed on the Na on pseudo-boehmite
+be locked in γ-Al
2o
3in lattice, thereby sodium element can not volatilize.And in traditional method, work as compounds containing sodium, as Na
2cO
3or Na
2c
2o
4, while being heated, can resolve into Na
2o, causes the loss of sodium.In the present invention, when applying thermal treatment, because being dissolved into, compounds containing sodium in solvent, forms Na
+, Na
+be adsorbed onto on pseudo-boehmite, compounds containing sodium can't resolve into Na
2o.Al element and Na and O direct reaction form β 〞-Al
2o
3.
Embodiment
Embodiment 1
Take 11.9g sodium salt and be dissolved in 100ml deionized water, vigorous stirring is until dissolve completely.In sodium nitrate solution, add 42.86g pseudo-boehmite powder, sonic oscillation 30min.Then under intense mechanical stirs, toward the dilute nitric acid solution that wherein drips 5mol/L, regulating PH is 4, continues to stir 3h, obtains the colloid of stable transparent.Adopt the dry colloid of spray-dryer to obtain xerogel.Atomization condition: colloid precursor flow 15mlmin
-1, 150 ℃ of hot air temperatures, 62 ℃ of material outlet temperature.By xerogel thermal treatment 3h at 600 ℃, remove organism, after using ethanol as medium ball milling 10h, obtain β 〞-Al
2o
3precursor powder.Measuring gained pottery specific conductivity at 300 ℃ is 0.013Scm
-1.
Embodiment 2
Take 11.9g sodium salt and be dissolved in 100ml deionized water, vigorous stirring is until dissolve completely.In sodium nitrate solution, add 42.86g pseudo-boehmite powder, sonic oscillation 30min.Then under intense mechanical stirs, toward the dilute nitric acid solution that wherein drips 5mol/L, regulating PH is 4, continues to stir 3h, obtains the colloid of stable transparent.Adopt the dry colloid of spray-dryer to obtain xerogel.Atomization condition: colloid precursor flow 15mlmin
-1, 150 ℃ of hot air temperatures, 62 ℃ of material outlet temperature.By xerogel thermal treatment 3h at 700 ℃, remove organism, after using ethanol as medium ball milling 10h, obtain β 〞-Al
2o
3precursor powder.
Embodiment 3
Take 11.9g sodium salt and be dissolved in 100ml deionized water, vigorous stirring is until dissolve completely.In sodium nitrate solution, add 42.86g pseudo-boehmite powder, sonic oscillation 30min.Then under intense mechanical stirs, toward the dilute nitric acid solution that wherein drips 5mol/L, regulating PH is 3, continues to stir 3h, obtains the colloid of stable transparent.Adopt the dry colloid of spray-dryer to obtain xerogel.Atomization condition: colloid precursor flow 15mlmin
-1, 150 ℃ of hot air temperatures, 62 ℃ of material outlet temperature.By xerogel thermal treatment 3h at 800 ℃, remove organism, after using ethanol as medium ball milling 10h, obtain β 〞-Al
2o
3precursor powder.
Claims (5)
1. the β 〞-Al of a high ion flux
2o
3the preparation method of precursor powder, is characterized in that comprising the following steps:
Step 1: appropriate sodium salt is dissolved in a certain amount of solvent, and vigorous stirring is until dissolving is completely made into sodium salt solution;
Step 2: appropriate pseudo-boehmite powder is mixed with certain proportion with deionized water, and ultrasonic dispersion 30min drips the dilute nitric acid solution of 5mol/L under intense mechanical stirs, and regulating PH is 2 ~ 4, continues to stir 3h, obtains Pseudo-boehmite;
Step 3: sodium salt solution is mixed with Pseudo-boehmite, and colloidal sol stirs to obtain;
Step 4: adopt the colloidal sol in spray-dryer drying step 3 to obtain xerogel;
Step 5: by xerogel thermal treatment 2 ~ 10h at 500 ℃ ~ 900 ℃, remove organism;
Step 6: as medium, the material that obtains of step 5 is carried out to ball milling 5 ~ 20h with ethanol, obtain β 〞-Al
2o
3precursor powder.
2. the β 〞-Al of a kind of high ion flux according to claim 1
2o
3the preparation method of precursor powder, its feature is NaNO at the sodium salt described in step 1
3, NaCOOCH
3, Na
2c
2o
4or Na
2sO
4.
3. a kind of β 〞-Al of high ion flux according to claim 1
2o
3the method of the preparation of precursor powder, is characterized in that step 1 solvent for use is deionized water.
4. the β 〞-Al of a kind of high ion flux according to claim 1
2o
3the preparation method of precursor powder, it is characterized in that keeping in step 3 in pseudo-boehmite mole proportioning of Na element in Al element and sodium salt is 4:1 ~ 11:1.
5. the β 〞-Al of a kind of high ion flux according to claim 1
2o
3the preparation method of precursor powder, is characterized in that in step 4, thermal treatment temp is 600 ~ 900 ℃.
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|---|---|---|---|
| CN201310128275.9A CN104098118A (en) | 2013-04-15 | 2013-04-15 | Preparation method for high-ion-flux beta''-Al2O3 precusor powder |
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|---|---|---|---|
| CN201310128275.9A CN104098118A (en) | 2013-04-15 | 2013-04-15 | Preparation method for high-ion-flux beta''-Al2O3 precusor powder |
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Family
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4797269A (en) * | 1988-02-08 | 1989-01-10 | Norton Company | Production of beta alumina by seeding and beta alumina produced thereby |
| CN1097351A (en) * | 1993-07-16 | 1995-01-18 | 中国石油化工总公司 | The preparation method of microspheroidal gama-alumina |
| CN101717259A (en) * | 2009-12-22 | 2010-06-02 | 中国科学院过程工程研究所 | Method for preparing Na-beta'-Al2O3 solid electrolyte precursor by adopting sol-gel method |
| CN101941835A (en) * | 2010-09-15 | 2011-01-12 | 张冰青 | Preparation method of Ba ion doped Na-beta'-Al2O3 solid electrolyte and solid electrolyte prepared by using same |
-
2013
- 2013-04-15 CN CN201310128275.9A patent/CN104098118A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4797269A (en) * | 1988-02-08 | 1989-01-10 | Norton Company | Production of beta alumina by seeding and beta alumina produced thereby |
| CN1097351A (en) * | 1993-07-16 | 1995-01-18 | 中国石油化工总公司 | The preparation method of microspheroidal gama-alumina |
| CN101717259A (en) * | 2009-12-22 | 2010-06-02 | 中国科学院过程工程研究所 | Method for preparing Na-beta'-Al2O3 solid electrolyte precursor by adopting sol-gel method |
| CN101941835A (en) * | 2010-09-15 | 2011-01-12 | 张冰青 | Preparation method of Ba ion doped Na-beta'-Al2O3 solid electrolyte and solid electrolyte prepared by using same |
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Application publication date: 20141015 |