CN1607611A - Sol-gel method for preparing cobalt ion doped titanium dioxide ferromagnetic material - Google Patents
Sol-gel method for preparing cobalt ion doped titanium dioxide ferromagnetic material Download PDFInfo
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- CN1607611A CN1607611A CN 200310105823 CN200310105823A CN1607611A CN 1607611 A CN1607611 A CN 1607611A CN 200310105823 CN200310105823 CN 200310105823 CN 200310105823 A CN200310105823 A CN 200310105823A CN 1607611 A CN1607611 A CN 1607611A
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Abstract
This invention relates to a preparation technology for a ferromagnetic material of Co ions doped with TiO2, especially to a chemical preparation technology for preparing Co ions doped with TiO2 particles and films by the sol-gel method. Compared with ordinary physical preparing method, this invented particles and films have uniform composition, the generation of nm Co particles is not discovered.
Description
Technical field this area relates to a kind of cobalt ion-doped titanic anhydride ferromagnetic material and technology of preparing thereof, particularly a kind of technology of preparing with Prepared by Sol Gel Method cobalt ion-doped titanic anhydride ferromagnetic particle and film.
Background technology titanium dioxide is a kind of epochmaking semiconductor functional material, has wide practical use in technical fields such as catalysis, photoelectricity, dielectrics.Particularly calendar year 2001, Y.Matsumoto etc. find that first the cobalt ion-doped titanic anhydride film at room temperature has ferromagnetism and semiconduting properties simultaneously, and this has advanced the dependence electron spin to carry out the development of quantum Storage technology greatly.Yet the technology of current preparation cobalt ion-doped titanic anhydride material mainly concentrates on the physical method, as laser molecular beam epitaxy sedimentation, magnetic control ion sputtering method etc.These methods can grow the film of uniaxial orientation, and the room temperature ferromagnetic of film and semiconduting properties are also better.But discover in the cobalt ion-doped titanic anhydride film with the physical method preparation more or less to have nano cobalt granule, its existence not only has influence on the semiconduting properties of film, and ferromagnetic source is produced ambiguity.In addition the desired technical sophistication of physical method, the cost bigger.
Summary of the invention the present invention overcomes the shortcoming that physical method prepares the cobalt ion-doped titanic anhydride material, providing a kind of has ferromagnetic and cobalt ion-doped titanic anhydride materials chemistry means semiconduting properties with the sol-gel method preparation, the particle of this method preparation and film composition evenly, do not find that nanometer cobalt metallic particles generates, the easy easy operating of while method, raw material be easy to get spend cheap.
Description of drawings
The XRD figure spectrum of the 5mol% cobalt ion-doped titanic anhydride particle of 500 ℃ of calcinings of Fig. 1
The XRD figure spectrum of the 5mol% cobalt ion-doped titanic anhydride particle of 700 ℃ of calcinings of Fig. 2
Embodiment is raw materials used to be had: the chemical pure tetrabutyl titanate, analyze pure absolute ethyl alcohol, and analyze pure cobalt nitrate or cobalt chloride, secondary deionized water.A certain amount of tetrabutyl titanate and a certain amount of absolute ethyl alcohol are mixed, as first component; A certain amount of cobalt nitrate or cobalt chloride and small amount of deionized water are dissolved in a certain amount of absolute ethyl alcohol as second component.Under agitation, second component is slowly splashed into acquisition avy blue solution in first component; Again this system is left standstill and to obtain vitreosol in 2 hours.This colloidal sol is divided into two parts, a copy of it leaves standstill in room temperature and obtained gel in 24 hours to 72 hours, this gel obtains xerogel 70 ℃ of following vacuumizes, the gel powder of xerogel after grinding put into high temperature resistance furnace calcine at a certain temperature a few hours get final product the cobalt ion-doped titanic anhydride particulate samples of crystallization.Will be in advance soaking with ethanol or acetone and the glass plate of ultrasonic cleaning or quartz glass plate impregnated among another part colloidal sol, adopt dipping-pulling method on glass plate or quartz glass plate, to obtain the cobalt ion-doped titanic anhydride film; Under certain humidity and temperature, keep 24 hours solvent flashings to finish gel simultaneously film, and put into high temperature resistance furnace calcine at a certain temperature a few hours get final product the cobalt ion-doped titanic anhydride film sample of crystallization.
The performance of implementation procedure of the present invention and material is by embodiment and description of drawings:
Embodiment one:
The absolute ethyl alcohol of 15 milliliters of tetrabutyl titanates and 20 milliliters is mixed, as first component; With 0.59 the gram cobalt nitrate and 0.2 ml deionized water be dissolved in 15 milliliters absolute ethyl alcohol in as second component.Under agitation, second component is slowly splashed into acquisition avy blue solution in first component; Again this system is left standstill and to obtain vitreosol in 2 hours, this colloidal sol is that 15-35 ℃, humidity are to leave standstill under the 30-60% condition to obtain gel in 24 hours to 72 hours in temperature, this gel obtains xerogel 70 ℃ of following vacuumizes, the gel powder of xerogel after grinding put into high temperature resistance furnace 500 ℃ of temperature lower calcinations got final product in 4 hours the cobalt ion-doped titanic anhydride particulate samples of crystallization.Fig. 1 has shown the XRD figure spectrum of the cobalt ion-doped titanic anhydride film particles of calcining.Fig. 1 has shown the XRD figure spectrum of the cobalt ion-doped titanic anhydride particle of calcining.
Embodiment two:
The absolute ethyl alcohol of 15 milliliters of tetrabutyl titanates and 20 milliliters is mixed, as first component; With 0.59 the gram cobalt nitrate and 0.2 ml deionized water be dissolved in 15 milliliters absolute ethyl alcohol in as second component.Under agitation, second component is slowly splashed into acquisition avy blue solution in first component; Again this system is left standstill and to obtain vitreosol in 2 hours, with soak with ethanol or acetone in advance and the glass plate of ultrasonic cleaning or the above-mentioned colloidal sol of quartz glass plate among dipping 1 minute, lift glass plate or quartz glass plate obtains the cobalt ion-doped titanic anhydride film with the speed of 10 cm per minute; Is that 15-35 ℃, humidity are to keep 24 hours solvent flashings to finish gel simultaneously under the 30-60% condition with this colloidal sol of film in temperature, and put into high temperature resistance furnace 500 ℃ down calcining got final product in 2 hours the cobalt ion-doped titanic anhydride film sample of crystallization.
Embodiment three:
The absolute ethyl alcohol of 15 milliliters of tetrabutyl titanates and 20 milliliters is mixed, as first component; With 0.59 the gram cobalt nitrate and 0.2 ml deionized water be dissolved in 15 milliliters absolute ethyl alcohol in as second component.Under agitation, second component is slowly splashed into acquisition avy blue solution in first component; Again this system is left standstill and to obtain vitreosol in 2 hours, this colloidal sol is that 15-35 ℃, humidity are to leave standstill under the 30-60% condition to obtain gel in 24 hours to 72 hours at this colloidal sol in temperature, this gel obtains xerogel 70 ℃ of following vacuumizes, the gel powder of xerogel after grinding put into high temperature resistance furnace 700 ℃ of temperature lower calcinations got final product in 4 hours the cobalt ion-doped titanic anhydride particulate samples of crystallization.Fig. 2 has shown the XRD figure spectrum of the cobalt ion-doped titanic anhydride particle of calcining.
Embodiment four:
The absolute ethyl alcohol of 15 milliliters of tetrabutyl titanates and 20 milliliters is mixed, as first component; In the absolute ethyl alcohol that cobalt nitrate and 0.2 milliliter of small amount of deionized water of 0.59 gram is dissolved in 15 milliliters as second component.Under agitation, second component is slowly splashed into acquisition avy blue solution in first component; Again this system is left standstill and to obtain vitreosol in 2 hours, with soak with ethanol or acetone in advance and the glass plate of ultrasonic cleaning or the above-mentioned colloidal sol of quartz glass plate among dipping 1 minute, lift glass plate or quartz glass plate obtains the cobalt ion-doped titanic anhydride film with the speed of 10 cm per minute; Is that 15-35 ℃, humidity are to keep 24 hours solvent flashings to finish gel simultaneously under the 30-60% condition with this colloidal sol of film in temperature, and put into high temperature resistance furnace 700 ℃ down calcining got final product in 2 hours the cobalt ion-doped titanic anhydride film sample of crystallization.
Claims (6)
1. to be the doping process begin and by normal temperature solgel reaction and calcining from solution for the sol-gel process for preparing of a cobalt ion-doped titanic anhydride ferromagnetic material, its principal character, the cobalt ions of realizing titanium dioxide evenly mix preparation ferromagnetic particle and film.
2. the sol-gel process for preparing of cobalt ion-doped titanic anhydride ferromagnetic material according to claim 1 is characterized in that the titanium source is titanium alkoxide (as tetrabutyl titanate, titanium propanolate, tetraethyl titanate) or titanium tetrachloride; Realize the doping of cobalt ions with cobalt nitrate or cobalt chloride.
3. the sol-gel process for preparing of cobalt ion-doped titanic anhydride ferromagnetic material according to claim 1, the preparation temperature that it is characterized in that collosol and gel are that 15-35 ℃, humidity are 30-60%.
4. the sol-gel process for preparing of cobalt ion-doped titanic anhydride ferromagnetic material according to claim 1, it is characterized in that in advance soaking and the glass plate of ultrasonic cleaning or quartz glass plate impregnated among the above-mentioned colloidal sol, adopt dipping-pulling method on glass plate or quartz glass plate, to obtain the cobalt ion-doped titanic anhydride film with ethanol or acetone.
5, the sol-gel process for preparing of cobalt ion-doped titanic anhydride ferromagnetic material according to claim 1 is characterized in that obtaining anatase and rutile particles material hot treatment temperature and is respectively 500 ℃ and 700 ℃, and the time is 4 hours.
6, the sol-gel process for preparing of cobalt ion-doped titanic anhydride ferromagnetic material according to claim 1, the heat treatment temperature that it is characterized in that obtaining anatase or rutile thin-film material is 500 ℃ and 700 ℃, the time is 2 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200310105823 CN1607611A (en) | 2003-10-13 | 2003-10-13 | Sol-gel method for preparing cobalt ion doped titanium dioxide ferromagnetic material |
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| CN 200310105823 CN1607611A (en) | 2003-10-13 | 2003-10-13 | Sol-gel method for preparing cobalt ion doped titanium dioxide ferromagnetic material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102765753A (en) * | 2012-07-15 | 2012-11-07 | 兰州理工大学 | Preparation method of nanometer TiO2 powder material with room-temperature ferromagnetism |
| CN106654246A (en) * | 2017-01-22 | 2017-05-10 | 福建师范大学 | Preparation method of circular porous TiO2 nanosheet and application thereof |
| WO2022116005A1 (en) * | 2020-12-01 | 2022-06-09 | 莱恩创科（北京）科技有限公司 | Titanium dioxide sterilization and disinfection film |
-
2003
- 2003-10-13 CN CN 200310105823 patent/CN1607611A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102765753A (en) * | 2012-07-15 | 2012-11-07 | 兰州理工大学 | Preparation method of nanometer TiO2 powder material with room-temperature ferromagnetism |
| CN106654246A (en) * | 2017-01-22 | 2017-05-10 | 福建师范大学 | Preparation method of circular porous TiO2 nanosheet and application thereof |
| CN106654246B (en) * | 2017-01-22 | 2019-01-25 | 福建师范大学 | A kind of rounded porous TiO2The preparation method and applications of nanometer sheet |
| WO2022116005A1 (en) * | 2020-12-01 | 2022-06-09 | 莱恩创科（北京）科技有限公司 | Titanium dioxide sterilization and disinfection film |
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