CN1588593A - Magnetic nano composite film and its method for preparing sol-gel - Google Patents
Magnetic nano composite film and its method for preparing sol-gel Download PDFInfo
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- CN1588593A CN1588593A CN 200410067150 CN200410067150A CN1588593A CN 1588593 A CN1588593 A CN 1588593A CN 200410067150 CN200410067150 CN 200410067150 CN 200410067150 A CN200410067150 A CN 200410067150A CN 1588593 A CN1588593 A CN 1588593A
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- film
- barium ferrite
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Abstract
The invention is a nano complex film and its sol-gel preparing method, firstly making a TiO2 sol and a barium ferrite precursor sol, respectively, then mixing them to make stable mixed sols in different mass proportions, adopting a rotating method to coat a substrate (like a quartz glass plate), making drying and thermal treatment to obtain a microcrack-free complex film. It belongs to a nano complex film and a crystal particle size less than 100 nm; it also belongs to an inorganic film and has a wide range of use temperature. It has higher magnetic property and has a wide application prospect in the fields of magnetic recording, electromagnetic screening, wave absorption coating, etc.
Description
Technical field
The present invention relates to a kind of nano compound film and preparation method thereof, relate in particular to a kind of magnetic nano-composite film and sol-gel process for preparing thereof, the laminated film that makes can be applicable to magnetic recording, electromagnetic shielding and microwave absorbing coating etc., belongs to technical field of function materials.
Background technology
Along with development of electronic technology, the application of electronic equipment is more prevalent, and almost the every nook and cranny all is flooded with electromagnetic wave.Electromagenetic wave radiation can not be out in the cold to ordinary production, life and health effects.Electromagenetic wave radiation effectively shielded and absorb becomes active demand.The first-selection that the thin film magnetic material is little with its thickness, light weight, application convenient and become research and use.Barium ferrite is a kind of magnetic material of excellent performance, has very strong magnetocrystalline anisotropy.Barium ferrite film is existing on magnetic recording, microwave equipment and electromagnetic shielding to be used widely.At present, the manufacture craft of barium ferrite film mainly contains two kinds: a kind of is to be millimetre-sized film [magnetic material and device, 27 (1996) 19～23] with being solidified into thickness after the polymer mixed such as ferrite powder and resin, and volume is bigger, and serviceability temperature is low; Another kind is to adopt sputtering method [functional material, 25 (1994) 172～175] and laser deposition [vacuum science and technology, 23 (2003) 195～199] to make single ferrite membrane, but the cost costliness, complicated operation.This type of film of making of sol-gal process has bigger stress, occurs micro-crack easily, and effect can not be satisfactory.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of magnetic nano-composite film and sol-gel process for preparing thereof are proposed, not only keep sol-gal process simple to operate, easily control chemical composition, can reach molecule rank benefits on uniformity, and the film surface that makes is even, flawless has higher serviceability temperature and magnetic.
For realizing such purpose, in the technical scheme of the present invention, make the precursor sol of TiO 2 sol and barium ferrite at first respectively, precursor sol with barium ferrite mixes mutually with TiO 2 sol then, make the stable mixed sols of different quality proportioning, adopt rotary process again, go up plated film at substrate (as quartz glass plate), after drying and the heat treatment, make non-microcracked laminated film.
The Prepared by Sol Gel Method technology of magnetic nano-composite film of the present invention mainly comprises the steps:
1, preparation contains the ethanolic solution of butyl titanate 0.5mol/L, stirs after 30 minutes, and the adding percent by volume is 4% diethanol amine and 0.8～1.0% deionized water; Continue to stir after 120 minutes, left standstill 120 minutes, obtain TiO 2 sol.
2, with mol ratio be 1: 12 Ba (NO
3)
2And Fe (NO
3)
39H
2O joins in 60 ℃ the ethylene glycol, makes Fe
3+Molar concentration be 1mol/L, treat to dissolve fully the back and add citric acid, making the molar concentration of citric acid in solution is 1.06mol/L, and dropwise add ethylenediamine to the pH of solution be 7.0, make citrate and Ba
2+, Fe
3+Fully complexing, the precursor sol of acquisition barium ferrite.
3, according to the barium ferrite mass ratio 1～3: 5 different, TiO 2 sol is mixed mutually the preparation mixed sols with the barium ferrite precursor sol with titanium dioxide.
4, adopt rotary process, with mixed sols plated film on the substrate of cleaning.
5, film was put into 60 ℃ of drying boxes dry 30 minutes.
6, dried film is put into Muffle furnace, be warming up to 850 ℃, be incubated 1 hour, cool to the furnace and obtain barium ferrite and titania coextruded film after the room temperature with 5 ℃/minute speed.
In the inventive method the barium ferrite precursor sol is mixed mutually with TiO 2 sol, because butyl titanate forms stable titanium dioxide network configuration when hydrolysis, so barium ferrite is just as embedding the titanium dioxide network.In dry and heat treatment process, the titanium dioxide network can be offset the internal stress of barium ferrite film to the constraint of barium ferrite, makes film micro-crack can not occur.Simultaneously, the mutual constraint of two kinds of materials has weakened moving of atom again, and crystal grain can not fully be grown up, thereby forms nano thin-film.
The butyl titanate that the present invention adopts can substitute with tetraethyl titanate or titanium propanolate.
The citric acid that the present invention adopts can substitute with glycine.
The laminated film of the present invention's preparation belongs to nano thin-film, is made up of barium ferrite and titanium dioxide, and the surface evenly, and is non-microcracked, has higher magnetic property, and the crystallite dimension in the film is all less than 100nm; Laminated film belongs to inoranic membrane, and the serviceability temperature scope is wide; Laminated film has higher magnetic property, is with a wide range of applications in fields such as magnetic recording, electromagnetic shielding and microwave absorbing coating.
Embodiment
Further describe technical scheme of the present invention below by specific embodiment.
Embodiment 1:
1, butyl titanate 1.1ml is joined in the 5ml absolute ethyl alcohol, stir after 30 minutes, add 0.25ml diethanol amine and 0.06ml deionized water, continue to stir 120 minutes, left standstill 120 minutes, obtain TiO 2 sol.
2, with 0.218gBa (NO
3)
2And 4.04gFe (NO
3)
39H
2O joins in 10ml60 ℃ the ethylene glycol, after the dissolving, adds the 2.218g citric acid fully.Dropwise adding ethylenediamine then, to make the pH of solution be 7.0, obtains the barium ferrite precursor sol.
3, sucking-off 0.6ml is added dropwise in the TiO 2 sol from above-mentioned barium ferrite precursor sol, fully stirs, and the mass ratio that obtains barium ferrite and titanium dioxide is 1: 5 a mixed sols.
4, adopt rotary process, with mixed sols plated film on quartz glass plate, rotating speed is 3000rmp, and the time is 15 seconds.
5, film was put into 60 ℃ of drying boxes dry 30 minutes.
6, dried film is put into Muffle furnace, be warming up to 850 ℃ with 5 ℃/minute speed, be incubated 1 hour, cooling to the furnace and obtaining barium ferrite and titanium dioxide mass ratio after the room temperature is 0.2 laminated film.Crystallite dimension in the film is less than 100nm, and film surface is even, and is non-microcracked, has higher magnetic property.
Embodiment 2:
1, titanium propanolate 0.87ml is joined in the 5ml absolute ethyl alcohol, stir after 30 minutes, add 0.23ml diethanol amine and 0.06ml deionized water, continue to stir 120 minutes, left standstill 120 minutes, obtain TiO 2 sol.
2, with 0.218gBa (NO
3)
2And 4.04gFe (NO
3)
39H
2O joins in 10ml60 ℃ 7 glycol, after the dissolving, adds the 2.218g citric acid fully.Dropwise adding ethylenediamine then, to make the pH of solution be 7.0, obtains the barium ferrite precursor sol.
3, sucking-off 1.2ml is added dropwise in the TiO 2 sol from above-mentioned barium ferrite precursor sol, fully stirs, and the mass ratio that obtains barium ferrite and titanium dioxide is 2: 5 a mixed sols.
4, adopt rotary process, with mixed sols plated film on quartz glass plate, rotating speed is 3000rmp, and the time is 15 seconds.
5, film was put into 60 ℃ of drying boxes dry 30 minutes.
6, dried film is put into Muffle furnace, be warming up to 850 ℃ with 5 ℃/minute speed, be incubated 1 hour, cooling to the furnace and obtaining barium ferrite and titanium dioxide mass ratio after the room temperature is 0.4 non-microcracked laminated film.
Embodiment 3:
1, tetraethyl titanate 0.65ml is joined in the 5ml absolute ethyl alcohol, stir after 30 minutes, add 0.22ml diethanol amine and 0.06ml deionized water, continue to stir 120 minutes, left standstill 120 minutes, obtain TiO 2 sol.
2, with 0.218gBa (NO
3)
2And 4.04gFe (NO
3)
39H
2O joins in 10ml60 ℃ the ethylene glycol, after the dissolving, adds the 2.377g glycine fully.Dropwise adding ethylenediamine then, to make the pH of solution be 7.0, obtains the barium ferrite precursor sol.
3, sucking-off 1.8ml is added dropwise in the TiO 2 sol from above-mentioned barium ferrite precursor sol, fully stirs, and the mass ratio that obtains barium ferrite and titanium dioxide is 3: 5 a mixed sols.
4, adopt rotary process, with mixed sols plated film on quartz glass plate, rotating speed is 3000rmp, and the time is 15 seconds.
5, film was put into 60 ℃ of drying boxes dry 30 minutes.
6, dried film is put into Muffle furnace, be warming up to 850 ℃ with the speed of 5 ℃/min, be incubated 1 hour, cooling to the furnace and obtaining barium ferrite and titanium dioxide mass ratio after the room temperature is 0.6 non-microcracked laminated film.
Claims (3)
1, a kind of magnetic nano-composite film and sol-gel process for preparing thereof is characterized in that comprising the steps:
1) preparation contains the ethanolic solution of butyl titanate 0.5mol/L, stirs after 30 minutes, adds percent by volume and be 4% diethanol amine and 0.8～1.0% deionized water, continues to stir after 120 minutes, leaves standstill the acquisition TiO 2 sol 120 minutes;
2) with mol ratio be 1: 12 Ba (NO
3)
2And Fe (NO
3)
39H
2O joins in 60 ℃ the ethylene glycol, makes Fe
3+Molar concentration be 1mol/L, treat to dissolve fully the back and add citric acid, making the molar concentration of citric acid in solution is 1.06mol/L, and dropwise add ethylenediamine to the pH of solution be 7.0, obtain the precursor sol of barium ferrite;
3), TiO 2 sol is pressed mass ratio 1～3 with the barium ferrite precursor sol: 5 mix mutually, the preparation mixed sols;
4) adopt rotary process, with mixed sols plated film on the substrate of cleaning;
5) film was put into 60 ℃ of drying boxes dry 30 minutes;
6) dried film is put into Muffle furnace, be warming up to 850 ℃, be incubated 1 hour, cool to the furnace and obtain barium ferrite and titania coextruded film after the room temperature with 5 ℃/minute speed.
2, the magnetic nano-composite film of claim 1 and sol-gel process for preparing thereof is characterized in that described butyl titanate substitutes with tetraethyl titanate or titanium propanolate.
3, claim 1 or 2 magnetic nano-composite film and sol-gel process for preparing thereof is characterized in that described citric acid substitutes with glycine.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410067150 CN1271652C (en) | 2004-10-14 | 2004-10-14 | Magnetic nano composite film and its method for preparing sol-gel |
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|---|---|---|---|
| CN 200410067150 CN1271652C (en) | 2004-10-14 | 2004-10-14 | Magnetic nano composite film and its method for preparing sol-gel |
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| CN1588593A true CN1588593A (en) | 2005-03-02 |
| CN1271652C CN1271652C (en) | 2006-08-23 |
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101599364B (en) * | 2009-07-01 | 2011-04-27 | 电子科技大学 | Method for preparing C axis orientation barium ferrite film |
| CN104129923A (en) * | 2013-05-05 | 2014-11-05 | 欧阳炜昊 | Preparation method of ferrite wave-absorbing membrane for preventing electromagnetic radiation of electrodeless lamp |
| CN104774590A (en) * | 2015-04-23 | 2015-07-15 | 京东方科技集团股份有限公司 | Composite material and preparation method thereof |
| CN106495228A (en) * | 2016-10-17 | 2017-03-15 | 王道远 | Nano combined alkaline earth permanent magnetism powder body and preparation method thereof |
| CN112323170A (en) * | 2020-10-16 | 2021-02-05 | 浙江义乌露炜针织内衣有限公司 | Antibacterial polyamide fiber for sock production and preparation method thereof |
| CN115216863A (en) * | 2021-06-18 | 2022-10-21 | 哈尔滨工业大学 | CoFe 2 O 4 -TiO 2 Composite fiber and preparation method and application thereof |
-
2004
- 2004-10-14 CN CN 200410067150 patent/CN1271652C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101599364B (en) * | 2009-07-01 | 2011-04-27 | 电子科技大学 | Method for preparing C axis orientation barium ferrite film |
| CN104129923A (en) * | 2013-05-05 | 2014-11-05 | 欧阳炜昊 | Preparation method of ferrite wave-absorbing membrane for preventing electromagnetic radiation of electrodeless lamp |
| CN104129923B (en) * | 2013-05-05 | 2016-09-14 | 欧阳炜昊 | The ferrite of a kind of anti-Non-polarized lamp electromagnetic radiation inhales the preparation method of ripple film |
| CN104774590A (en) * | 2015-04-23 | 2015-07-15 | 京东方科技集团股份有限公司 | Composite material and preparation method thereof |
| US9873773B2 (en) | 2015-04-23 | 2018-01-23 | Boe Technology Group Co., Ltd. | Composite material and method for preparing the same |
| CN106495228A (en) * | 2016-10-17 | 2017-03-15 | 王道远 | Nano combined alkaline earth permanent magnetism powder body and preparation method thereof |
| CN112323170A (en) * | 2020-10-16 | 2021-02-05 | 浙江义乌露炜针织内衣有限公司 | Antibacterial polyamide fiber for sock production and preparation method thereof |
| CN112323170B (en) * | 2020-10-16 | 2023-04-07 | 浙江义乌露炜针织内衣有限公司 | Antibacterial polyamide fiber for sock production and preparation method thereof |
| CN115216863A (en) * | 2021-06-18 | 2022-10-21 | 哈尔滨工业大学 | CoFe 2 O 4 -TiO 2 Composite fiber and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN1271652C (en) | 2006-08-23 |
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Granted publication date: 20060823 Termination date: 20091116 |