CN104556216A - Method for preparing barium titanate nanopowder by adopting non-hydrolytic sol-gel process - Google Patents
Method for preparing barium titanate nanopowder by adopting non-hydrolytic sol-gel process Download PDFInfo
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Abstract
The invention discloses a method for preparing barium titanate nanopowder by adopting a non-hydrolytic sol-gel process. The method comprises the following steps: dissolving an anhydrous barium source and an anhydrous titanium source into anhydrous low-carbon alcohol, performing uniform stirring, and performing non-hydrolytic condensation reaction to obtain precursor sol by virtue of oil-bath refluxing; drying the precursor sol, adding a mineralizing agent, and performing uniform mixing, calcination and washing to obtain the barium titanate nanopowder. The method has the outstanding advantages of simple preparation process, low synthesis temperature, short cycle, high crystal grain dispersibility and the like, so that the method has broad application prospect.
Description
Technical field
The invention belongs to technical field of inorganic nonmetallic materials, be specifically related to a kind of method adopting non-hydrolytic sol-gel process to prepare Barium Titanate nano-powder.
Background technology
Barium titanate is a kind of important perovskite type ferroelectric material, because it has high specific inductivity, and the performances such as excellent ferroelectric, piezoelectricity, thus become the main raw material manufacturing electronic ceramics, be widely used in laminated ceramic capacitor, thermistor etc.Along with electronic component is to the development in micro-, thin, light direction, require the number of plies of multilayer ceramic capacitor medium layer constantly to increase and the lasting reduction of the thickness of medium layer, therefore for preparing, grain-size is little, particle size distribution range is narrow, the demand of the Barium Titanate nano-powder of good dispersity is growing.
The method preparing barium carbonate powder at present mainly contains solid phase method, hydrothermal method, coprecipitation method, hydrolytic sol-gel process, non-hydrolytic sol-gel process etc.It is high that solid phase method prepares barium carbonate powder synthesis temperature, and crystal grain is large and size distribution is wide, easily introduces impurity.Hydrothermal method needs under high pressure to carry out, higher to equipment requirements, makes the method be difficult to promote.When coprecipitation method prepares barium carbonate powder, because the throw out solubility product constant of barium and titanium differs greatly, be difficult to form uniform throw out, and particle is easily reunited, size distribution is wide, unstable product quality.Prepare in barium carbonate powder at hydrolytic sol-gel process, the metal alkoxide that general employing is expensive or metal inorganic salt are presoma, because different presoma hydrolysis rate there are differences, therefore need strict Controlling Technology condition.S.B. the people such as Deshpande with barium carbonate and butyl (tetra) titanate for barium source and titanium source, glacial acetic acid, isopropyl alcohol and water are solvent, adopt hydrolytic sol-gel process synthesized at 750 DEG C barium carbonate powder (see Journal of Electroceramics, 15,103-108,2005); The people such as Yao Yanyan adopt hydrolytic sol-gel process; with the barium metal of costliness (for synthesizing barium alkoxides with ethylene glycol monomethyl ether under the condition of 0 DEG C of water-bath and nitrogen protection), for barium source, butyl (tetra) titanate is titanium source, has synthesized barium titanate (see silicate journal at 150 DEG C; 2004; Vol.32, P751-754), because barium is heavy metal element; and in the Nature, never found the existence of simple substance barium; so method cost of material is high, technology condition complexity is high, not easily promotes.
Non-hydrolytic sol-gel process be the nineties in last century France professor Corriu wait a kind of wet chemical method proposed, it is characterized in that without metal alkoxide hydrolytic process, is directly gel by reactant polycondensation.Compared with conventional hydrolysis sol-gel (HSG) method, the method not only simplify technological process, avoid with water is the reunion that solvent causes, the more important thing is and be easy to realize atom level Homogeneous phase mixing in sol-gel process, greatly can reduce the synthesis temperature of oxide compound, have broad application prospects in the preparation of barium titanate and barium titanate doping powder.The people such as Chaoliang Mao adopt non-hydrolytic sol-gel process to prepare barium-strontium titanate powder (see Ceramics International, 2008, Vol.34, P45 – 49), its method is dissolved in acetic acid by barium acetate, butyl (tetra) titanate dissolves in ethanol, after mixing, add a certain amount of acetone, it is heated in about 50 DEG C water-baths 10 h and obtain precursor sol, colloidal sol is placed in 120 DEG C of dry 12 h of baking oven and obtains dry gel powder, dry gel powder is sintered into barium-strontium titanate powder through 800 DEG C.But because the solvent acetic acid being used for dissolving barium acetate is strong lewis acid, be easy to the polymerization of catalysis butyl (tetra) titanate generation homogeneity, be difficult to form heteropolymerization, this is also the basic reason of its synthesis temperature up to 800 DEG C (not detecting Ba-O-Ti bonding in xerogel infared spectrum).Therefore preparation method's technique of barium carbonate powder is more complicated at present, synthesis temperature is higher, is not suitable for large industrial production and uses.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method that raw material sources are extensive, preparation technology is simple, production cost is low, employing non-hydrolytic sol-gel process prepares Barium Titanate nano-powder.
For solving above technical problem, technical scheme of the present invention is: a kind of method adopting non-hydrolytic sol-gel process to prepare Barium Titanate nano-powder, comprises following steps:
(1) by appropriate anhydrous barium source, low-carbon alcohol mixing, heated and stirred obtains solution A;
(2) appropriate anhydrous titanium source is dissolved in low-carbon alcohol obtains solution B, then solution B is joined in above-mentioned solution A, uniform stirring, obtain transparent mixed solution C;
(3) mixed solution C obtains barium titanate precursor sol D after oil bath backflow, adds appropriate mineralizer after being dried, and through ball milling, calcining, washing obtains Barium Titanate nano-powder.
Described anhydrous barium source is anhydrous formic acid barium, anhydrous acetic acid barium.
Described anhydrous titanium source is butyl (tetra) titanate, titanium isopropylate, titanium ethanolate.
The carbon atom number of described low-carbon alcohol is 1 ~ 4.
The concentration of described mixed solution C is 0.5 ~ 1.0 mol/L.
Described oil bath reflux temperature is 100 ~ 180 DEG C, and oil bath return time is 24 ~ 48 h.
Described drying temperature is 130 ~ 260 DEG C.
Described mineralizer is potassium vanadate, vanadic acid sodium.
The mol ratio of mineralizer and barium titanate dry gel powder consumption is 0 ~ 0.04.
Described calcining temperature is 550 ~ 650 DEG C.
Above-mentioned reactive chemistry equation is as follows:
The present invention causes non-hydrolytic polycondensation in non-aqueous system, form Ba-O-Ti heteropolymerization, the synthesis temperature of Barium Titanate nano-powder is made to be reduced to 650 DEG C, also introduce alkali metal vanadate innovatively as mineralizer simultaneously, the temperature of non-hydrolytic sol-gel process synthesis of barium titanate nano-powder is made to be reduced to 550 DEG C further, there is the outstanding advantages such as preparation technology is simple, synthesis temperature is low, the cycle is short, grain dispersion is good, therefore there is the wide market space.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that non-hydrolytic sol-gel process prepares Barium Titanate nano-powder.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Embodiment 1
With anhydrous acetic acid barium (analytical pure), butyl (tetra) titanate (analytical pure) is presoma, take ethanol (analytical pure) as the solvent dissolving anhydrous acetic acid barium and butyl (tetra) titanate.First, the anhydrous acetic acid barium taking 0.025 mol in glove box is placed in dry Erlenmeyer flask, then adds the alcohol solvent of 40 ml, heated and stirred.The butyl (tetra) titanate measuring 0.025 mol is dissolved in the ethanol of 16.7 ml, is uniformly mixed.By titanium source and the mixing of barium source, continue to stir.Oil bath pan mixing solutions being placed in 100 DEG C 24 h that reflux obtain barium titanate precursor solution, dry at precursor solution being placed in 130 DEG C, calcined by dry gel powder, obtain Barium Titanate nano-powder at 650 DEG C.
Embodiment 2
With anhydrous acetic acid barium (analytical pure), butyl (tetra) titanate (analytical pure) is presoma, take ethanol (analytical pure) as the solvent dissolving anhydrous acetic acid barium and butyl (tetra) titanate.Prepare barium carbonate powder technical process used and experiment condition identical with embodiment 1, just add mineralizer potassium vanadate after drying, the mol ratio of the amount added and barium titanate dry gel powder amount is 0.01, and through 550 DEG C of calcinings after ball milling, washing obtains Barium Titanate nano-powder.
Embodiment 3
With anhydrous acetic acid barium (analytical pure), titanium ethanolate (analytical pure) is presoma, take Virahol (analytical pure) as the solvent dissolving barium acetate and titanium ethanolate.Prepare barium carbonate powder technical process used and experiment condition identical with embodiment 1.Just oil bath temperature is 120 DEG C, and reflux 36 h, and drying temperature is 150 DEG C, adds potassium vanadate mineralizer after drying, and the mol ratio of the amount added and barium titanate dry gel powder amount is 0.02, and through 600 DEG C of calcinings after ball milling, washing obtains Barium Titanate nano-powder.
Embodiment 4
With anhydrous acetic acid barium (analytical pure), butyl (tetra) titanate (analytical pure) is presoma, take butanols (analytical pure) as the solvent dissolving barium acetate, and methyl alcohol (analytical pure) is the solvent dissolving butyl (tetra) titanate.Prepare barium carbonate powder technical process used and experiment condition identical with embodiment 1.Just oil bath temperature is 140 DEG C, and reflux 24 h, and drying temperature is 170 DEG C, adds vanadic acid sodium mineralizer after drying, and the mol ratio of the amount added and barium titanate dry gel powder amount is 0.02, and through 600 DEG C of calcinings after ball milling, washing obtains Barium Titanate nano-powder.
Embodiment 5
With anhydrous acetic acid barium (analytical pure), titanium isopropylate (analytical pure) is presoma, take ethanol (analytical pure) as the solvent dissolving barium acetate, and butanols (analytical pure) is the solvent dissolving titanium isopropylate.Prepare barium carbonate powder technical process used and experiment condition identical with embodiment 1.Just oil bath temperature is 160 DEG C, and reflux 48 h, and drying temperature is 190 DEG C, adds potassium vanadate mineralizer after drying, and the mol ratio of the amount added and barium titanate dry gel powder amount is 0.03, and through 600 DEG C of calcinings after ball milling, washing obtains Barium Titanate nano-powder.
Embodiment 6
With anhydrous formic acid barium (analytical pure), titanium isopropylate (analytical pure) is presoma, take methyl alcohol (analytical pure) as the solvent dissolving barium formate and titanium isopropylate.Prepare barium carbonate powder technical process used and experiment condition identical with embodiment 1.Just oil bath temperature is 160 DEG C, and reflux 36 h, and drying temperature is 200 DEG C, adds vanadic acid sodium mineralizer after drying, and the mol ratio of the amount added and barium titanate dry gel powder amount is 0.03, and through 650 DEG C of calcinings after ball milling, washing obtains Barium Titanate nano-powder.
Embodiment 7
With anhydrous formic acid barium (analytical pure), butyl (tetra) titanate (analytical pure) is presoma, take glycerol (analytical pure) as the solvent dissolving barium formate, and butanols (analytical pure) is the solvent dissolving butyl (tetra) titanate.Prepare barium carbonate powder technical process used and experiment condition identical with embodiment 1.Just oil bath temperature is 180 DEG C, and reflux 24 h, and drying temperature is 240 DEG C, adds potassium vanadate mineralizer after drying, and the mol ratio of the amount added and barium titanate dry gel powder amount is 0.03, and through 600 DEG C of calcinings after ball milling, washing obtains Barium Titanate nano-powder.
Embodiment 8
With anhydrous formic acid barium (analytical pure), titanium ethanolate (analytical pure) is presoma, take glycerol (analytical pure) as the solvent dissolving barium formate and titanium ethanolate.Prepare barium carbonate powder technical process used and experiment condition identical with embodiment 1.Just oil bath temperature is 180 DEG C, and reflux 36 h, and drying temperature is 260 DEG C, adds vanadic acid sodium mineralizer after drying, and the mol ratio of the amount added and barium titanate dry gel powder amount is 0.04, and through 650 DEG C of calcinings after ball milling, washing obtains Barium Titanate nano-powder.
Claims (10)
1. adopt non-hydrolytic sol-gel process to prepare a method for Barium Titanate nano-powder, comprise following steps:
(1) by appropriate anhydrous barium source, low-carbon alcohol mixing, heated and stirred obtains solution A;
(2) appropriate anhydrous titanium source is dissolved in low-carbon alcohol obtains solution B, then solution B is joined in above-mentioned solution A, uniform stirring, obtain transparent mixed solution C;
(3) mixed solution C obtains barium titanate precursor sol D after oil bath backflow, adds appropriate mineralizer after being dried, and through ball milling, calcining, washing obtains Barium Titanate nano-powder.
2. prepare the method for Barium Titanate nano-powder according to claim 1, it is characterized in that: described anhydrous barium source is anhydrous formic acid barium, anhydrous acetic acid barium.
3. prepare the method for Barium Titanate nano-powder according to claim 1, it is characterized in that: described anhydrous titanium source is butyl (tetra) titanate, titanium isopropylate, titanium ethanolate.
4. prepare the method for Barium Titanate nano-powder according to claim 1, it is characterized in that: the carbon atom number of described low-carbon alcohol is 1 ~ 4.
5. prepare the method for Barium Titanate nano-powder according to claim 1, it is characterized in that: the concentration of described mixed solution C is 0.5 ~ 1.0 mol/L.
6. prepare the method for Barium Titanate nano-powder according to claim 1, it is characterized in that: described oil bath reflux temperature is 100 ~ 180 DEG C, oil bath return time is 24 ~ 48 h.
7. prepare the method for Barium Titanate nano-powder according to claim 1, it is characterized in that: described drying temperature is 130 ~ 260 DEG C.
8. prepare the method for Barium Titanate nano-powder according to claim 1, it is characterized in that: described mineralizer is potassium vanadate, vanadic acid sodium.
9. prepare the method for Barium Titanate nano-powder according to claim 1, it is characterized in that: the mol ratio of mineralizer and barium titanate dry gel powder consumption is 0 ~ 0.04.
10. prepare the method for Barium Titanate nano-powder according to claim 1, it is characterized in that: described calcining temperature is 550 ~ 650 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106380195A (en) * | 2016-10-08 | 2017-02-08 | 东北大学 | Bariumtitanate ceramic and preparation method thereof |
| CN106752142A (en) * | 2016-12-16 | 2017-05-31 | 安徽宝恒新材料科技有限公司 | A kind of preparation method of easy cutting stainless steel plate |
| CN110252306A (en) * | 2019-07-19 | 2019-09-20 | 景德镇陶瓷大学 | A kind of novel recyclable Fe2TiO5The preparation method and applications of/C composite visible light catalytic material |
| CN115135606A (en) * | 2020-02-27 | 2022-09-30 | 东南大学 | Method for preparing tetragonal phase barium titanate nano particles |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110252306A (en) * | 2019-07-19 | 2019-09-20 | 景德镇陶瓷大学 | A kind of novel recyclable Fe2TiO5The preparation method and applications of/C composite visible light catalytic material |
| CN110252306B (en) * | 2019-07-19 | 2021-10-29 | 景德镇陶瓷大学 | Recoverable Fe2TiO5Preparation method and application of/C composite visible light catalytic material |
| CN115135606A (en) * | 2020-02-27 | 2022-09-30 | 东南大学 | Method for preparing tetragonal phase barium titanate nano particles |
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