CN102592836A - Process for preparing iron-doped titanium dioxide powders - Google Patents
Process for preparing iron-doped titanium dioxide powders Download PDFInfo
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- CN102592836A CN102592836A CN2012100258601A CN201210025860A CN102592836A CN 102592836 A CN102592836 A CN 102592836A CN 2012100258601 A CN2012100258601 A CN 2012100258601A CN 201210025860 A CN201210025860 A CN 201210025860A CN 102592836 A CN102592836 A CN 102592836A
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Abstract
The invention discloses a process for preparing iron-doped titanium dioxide powder materials through a sol-gel method. The process includes five reaction processes and has the advantages of having low raw material cost, mild reaction conditions, low energy consumptions and having no coarse particle aggregation members produced and the like. According to the process for preparing iron-doped titanium dioxide powder materials, the iron-doped titanium dioxide powder materials enable the sunlight induction range to be expanded and enable the sunlight absorption wavelength to perform a redshift and have a good prospect in manufacturing the electrodes of the solar battery.
Description
Technical field
The present invention relates to a kind of preparation technology of iron doped titanium dioxide powder.
Background technology
Titanium dioxide becomes the photochemical catalyst of tool application potential owing to its good chemical stability, abrasion resistance, low cost, characteristics such as nontoxic.But owing to receive the restriction of energy gap, titanium dioxide is lower to the utilance of sunlight.TiO
2Belong to wide bandgap semiconductor, the ability of catching sunlight is relatively poor, mainly is at present to adopt the method for dye sensitization to prepare the Optical Electro-Chemistry solar cell with broad spectral absorption scope.The titanium dioxide electrodes material requires than higher the selection of sensitizer, and is bigger to the selection aspect dependence of sensitizer, improved production cost.Report was constantly arranged in recent years, an amount of transient metal doped Ti0 again
2Can introduce defective locations on its surface, become the trap of electronics or defective, reduce the compound of electronics and hole, enlarge induction light district scope, the photoelectric conversion efficiency that improves battery is had positive role.
Iron is titania-doped to be that semiconductor is material modified, relevant report is verified its in the catalytic degradation extensive applications.People such as Bao Nan have proposed a kind of preparation method of nano titanic oxide catalyst in " functional material and device journal " (the 14th volume the 2nd phase 462-466 page or leaf April in 2008) " the preparation of ultrasound templates method and photocatalytic activity thereof that the iron doping titanium dioxide nano is brilliant " literary composition; It is a raw material with butyl titanate and ferric nitrate; And be aided with lauryl amine and make template; Sonochemical method is combined with mould plate technique, prepared serial iron doped Ti O
2Nanocrystalline.Use this method can make the anatase type nano crystal that particle diameter is even, form is regular, pattern is orderly, and can realize that ferro element mixes uniformly and effectively.But control reaction system at 80 ℃ and use high-energy ultrasound (4 hours) for a long time because this method prepares in the process needs, energy consumption is bigger, and industrial production cost is than higher.In addition; People such as He Dannong disclose a kind of porous iron-doped titanic oxide Preparation of catalysts method (number of patent application 200810042475.1; Notification number CN101347732B), it may further comprise the steps: in ethylene glycol solvent, add solid Iron(III) chloride hexahydrate FeCl successively
36H
2O and butyl titanate Ti (OC
4H
9)
4, carry out stirring and refluxing and be cooled to room temperature; Place centrifuge to separate cooled solution again, be placed on then and carry out several times dispersion and cleaning in the absolute ethyl alcohol, obtain the metal alkoxide solid; After carrying out dried and heat treated, obtain the pressed powder of porous iron-doped titanic oxide photocatalyst.Use the porous iron-doped titanic oxide photocatalyst of this method preparation in the reaction of degradable organic pollutant molecule, to have higher photocatalytic activity; But the transmission electron microscope photo that provides from this application; About 250～the 500nm of bar-shaped titanium dioxide diameter that it obtains; The nearly 10 μ m of length, size is bigger than normal, is inappropriate for the electrode of solar battery material.
Summary of the invention
The objective of the invention is for overcoming the deficiency of above-mentioned prior art, the present invention is devoted to the improvement to titania modified technology, and a kind of titania-doped optimization synthesis technique of iron for preparing is provided.
For realizing above-mentioned purpose, the present invention adopts following technical proposals:
1. the preparation technology of an iron doped titanium dioxide powder is characterized in that, comprises following step:
(1), adds hydrolysis inhibitor and obtain the homogeneous transparent solution A with adding absolute ethyl alcohol in the butyl titanate;
(2) mol ratio according to Ti and Fe is (20-5): 1, and with FeCl
36H
2O is dissolved in the absolute ethyl alcohol, forms FeCl
3Alcoholic solution B;
(3) at room temperature, solution B is joined in the solution A slowly stirred in the time of dropping, obtains the solution C of homogeneous transparent;
(4) solution C is stirred 15-30 minute after, leave standstill and carry out dried and obtain xerogel;
(5) xerogel is carried out heat treated and make the iron doped titanium dioxide powder.
The volume ratio of said butyl titanate and absolute ethyl alcohol is 1: 1-1: 2.
Said hydrolysis inhibitor is a glacial acetic acid, the volume ratio 10 of butyl titanate and glacial acetic acid: 1-10: 2.Glacial acetic acid is a hydrolysis inhibitor, and the crystallization water of can the bound fraction iron chloride hexahydrate bringing into reduces the content of the Free water in the solution, slows down hydrolysis rate, avoids forming macroaggregate.
Said step (1) is specially: under the room temperature, butyl titanate is under agitation slowly splashed in the beaker that fills ethanol, when stirring, slowly add glacial acetic acid, continue to stir the solution A that obtains homogeneous transparent.
FeCl in the said step (2)
36H
2The mass percent that O accounts for absolute ethyl alcohol is 3-15%.
The solution C time of repose is to leave standstill under the first room temperature 2 days in the said step (4), obtains yellow wet gel, places 48-72 hour naturally under the room temperature then.
Dried is in the said step (4): solution C leaves standstill the back dries in temperature is set to 110-130 ℃ baking oven.
Said step (5) is: xerogel is ground to form evengranular powder, be placed in the Muffle furnace calcination 2-5 hour, it is 200-700 ℃ that temperature is set.Here carry out the setting of temperature according to the report of pertinent literature and the demand of experiment,, the variation of crystal formation can take place because at a certain temperature material modified, different crystal formations, for example rutile-type and Detitanium-ore-type, its photoelectric conversion efficiency is obviously different.
Said calcination temperature is 200-500 ℃, and obtaining crystal formation is anatase sections doped titanium dioxide powder.
Said calcination temperature is 550-700 ℃, the iron doped titanium dioxide powder that obtains crystal formation and be rutile-type and Detitanium-ore-type and deposit.
The present invention is predecessor with the butyl titanate, through Prepared by Sol Gel Method iron doped titanium dioxide powder.Comprise producing of (1) butyl titanate alcoholic solution; (2) the ferric trichloride alcoholic solution produces; (3) powder gel mother liquor produces; (4) the powder xerogel produces; (5) make the iron doped titanium dioxide powder by xerogel.
Present patent application in the preparation procedure of titanium dioxide doping gel with background technology in the difference of two kinds of schemes be: (1) reduces reaction temperature, makes most of reaction at room temperature, reduces energy consumption, practices thrift cost; (2) use hydrolysis inhibitor, do not add distilled water, slow down hydrolysis rate, avoid the generation of macroaggregate.
The beneficial effect of technology of the present invention is: (1) low in raw material cost is easy to get, and can reduce cost; (2) reaction condition is gentle, and most of reactions step is at room temperature carried out, and energy consumption is low, practices thrift cost; (3) do not add distilled water, use hydrolysis inhibitor, slow down hydrolysis rate, do not produce macroaggregate.
The product that uses this technology to obtain is mainly anatase titanium dioxide, has been extended to 500nm through measuring its maximum induction wavelength by 398nm, thereby has expanded the induction range to sunlight, improves solar energy utilization rate.This material can be used as the preparation raw material of electrode of solar battery, when suppressing electronics-hole-recombination, improves the photoelectric conversion efficiency of battery.
Description of drawings
Fig. 1: doped Ti O not
2The EDS power spectrum;
Fig. 2: iron doped Ti O
2The EDS power spectrum;
Fig. 3: doped Ti O not
2Uv-visible absorption spectra figure;
Fig. 4: iron doped Ti O
2Uv-visible absorption spectra figure;
Fig. 5: Detitanium-ore-type TiO
2X-ray diffractogram of powder;
Fig. 6: Detitanium-ore-type and rutile-type are also deposited the x-ray diffractogram of powder of titanium dioxide.
Embodiment
Through instantiation the present invention is further set forth below, should be noted that following explanation only is in order to explain the present invention, its content not to be limited.
Embodiment 1:
(1) under agitation the 10ml butyl titanate is slowly splashed into the 50ml beaker that fills the 10ml absolute ethyl alcohol, after dropwising, under agitation continue to drip the 1ml glacial acetic acid, vigorous stirring obtained the solution A of homogeneous transparent in 30 minutes.
(2) take by weighing 0.49g FeCl
36H
2O, Fe and Ti mol ratio are 20: 1, add 5ml ethanol, dissolve under the room temperature, obtain containing FeCl
3Solution B.
(3) under the room temperature, solution B is gently dropwise joined solution A, under agitation drip the solution C that obtains homogeneous transparent.
(4) stir after 30 minutes, stop to stir, at room temperature the solution C that obtains was left standstill 2 days, obtain yellow wet gel, place naturally under the room temperature 72 little after, putting into temperature is set is that 110 ℃ baking oven is dried.
(5) xerogel that obtains is ground to form evengranular powder, be placed on calcination in the Muffle furnace, it is 200 ℃ that temperature is set, and calcination time is 2 hours.
Test obtain material modified through XRD, crystal formation is a Detitanium-ore-type, sees accompanying drawing 5.
In the preparation process, observe, after stirring, do not observe the formation of macroaggregate in the infall process; And add after the distilled water in addition; The content of free water is excessive, can cause the too fast formation macroaggregate of hydrolysis, influences the homogeneous and the transparency of titania gel.Mainly show as the adularescent particle and appear in the gel, out-of-shape is about diameter 2mm.
To prepare scheme not identical for the titanium dioxide powder of producing in the scheme taked is published in solar energy journal with Qin Haoli the article " research of Prepared by Sol Gel Method nitrogen-doped titanium dioxide and visible light activity thereof " of titania-doped Comparative Examples.
Like Fig. 1, shown in Figure 2, the iron doped titanium dioxide powder of preparation to be compared with doped titanium dioxide powder not, the conclusion that Fig. 1 and Fig. 2 can draw is: ferro element has got into titanium dioxide crystal lattice, rather than exists with independent oxide form.
Like Fig. 3, shown in Figure 4, can find out: maximum induction wavelength has been extended to 500nm by 398nm, thereby expands the induction range to sunlight, improves solar energy utilization rate.
Embodiment 2:
(1) under agitation the 10ml butyl titanate is slowly splashed into the 50ml beaker that fills the 10ml absolute ethyl alcohol, after dropwising, under agitation continue to drip the 1.0ml glacial acetic acid, vigorous stirring obtained the solution A of homogeneous transparent in 30 minutes;
(2) take by weighing 0.98g FeCl
36H
2O, Fe and Ti mol ratio are 10: 1, add 5ml ethanol, dissolve under the room temperature, obtain containing FeCl
3Solution B.
(3) under the room temperature, with solution B slowly dropwise join solution A, under agitation drip the solution C that obtains homogeneous transparent.
(4) stir after 15 minutes, stop to stir, at room temperature the solution C that obtains was left standstill 2 days, obtain yellow wet gel, place after 72 hours naturally under the room temperature, putting into temperature is set is that 110 ℃ baking oven is dried.
(5) xerogel that obtains is ground to form evengranular powder, be placed on calcination in the Muffle furnace, it is 300 ℃ that temperature is set, and calcination time is 2 hours.
Test obtain material modified through XRD, crystal formation is a Detitanium-ore-type.
Embodiment 3:
(1) under agitation the 10ml butyl titanate is slowly splashed into the 50ml beaker that fills the 10ml absolute ethyl alcohol, after dropwising, under agitation continue to drip the 1ml glacial acetic acid, vigorous stirring obtained the solution A of homogeneous transparent in 30 minutes.
(2) take by weighing 1.96gFeCl36H2O, Fe and Ti mol ratio are 5: 1.Add 5ml ethanol, dissolve under the room temperature, obtain containing the solution B of FeCl3.
(3) under the room temperature, solution B is gently dropwise joined solution A, all dropwise, obtain the solution C of homogeneous transparent, continue to stir while stir.
(4) stir after 20 minutes, stop to stir, at room temperature the solution C that obtains was left standstill 2 days, obtain yellow wet gel, place after 72 hours naturally under the room temperature, putting into temperature is set is that 110 ℃ baking oven is dried.
(5) xerogel that obtains is ground to form evengranular powder, be placed on calcination in the Muffle furnace, it is 500 ℃ that temperature is set, and calcination time is 3 hours.Test obtain material modified through XRD, crystal formation is a Detitanium-ore-type.
Embodiment 4:
(1) under agitation the 10ml butyl titanate is slowly splashed into the 100ml beaker that fills the 10ml absolute ethyl alcohol, after dropwising, under agitation continue to drip the 1ml glacial acetic acid, vigorous stirring obtained the solution A of homogeneous transparent in 30 minutes.
(2) take by weighing 1.96g FeCl36H2O, add 10ml ethanol, dissolve under the room temperature, obtain containing the solution B of FeCl3.
(3) under the room temperature, solution B is gently dropwise joined solution A, under agitation drip the solution C that obtains homogeneous transparent.
(4) stir after 30 minutes, stop to stir, at room temperature the solution C that obtains was left standstill 2 days, obtain yellow wet gel, place after 72 hours naturally under the room temperature, putting into temperature is set is that 130 ℃ baking oven is dried.
(5) xerogel that obtains is ground to form evengranular powder, be placed on calcination in the Muffle furnace, it is 700 ℃ that temperature is set, and calcination time is 3 hours.
Test obtain material modified through XRD, the powder body material crystal formation is Detitanium-ore-type and rutile-type and deposits, sees accompanying drawing 6.
Embodiment 5:
(2), (3), (5) are with embodiment one, (1) is located to change under agitation the 10ml butyl titanate is slowly splashed into the 50ml beaker that fills the 20ml absolute ethyl alcohol, (5) are located the Muffle furnace calcination temperature and are set to 300 ℃, calcination time is 2 hours.Test obtain material modified through XRD, the powder body material that obtains is mainly anatase phase titanium dioxide, sees accompanying drawing 5.
Embodiment 6:
(2), (3), (5) are with embodiment two; (1) locates to change under agitation the 10ml butyl titanate is slowly splashed into the 50ml beaker that fills the 20ml absolute ethyl alcohol; (5) locate the Muffle furnace calcination temperature and be set to 200 ℃; Calcination time is 3 hours, tests obtain material modified through XRD, and the powder body material that obtains is mainly anatase phase titanium dioxide.
Embodiment 7:
(1), (2), (3), (4) are with embodiment three, (5) are located the Muffle furnace calcination temperature and are set to 400 ℃, calcination time is 4 hours.Test obtain material modified through XRD, the powder body material that obtains is mainly anatase phase titanium dioxide.
Embodiment 8:
(1), (2), (3), (4) are with embodiment three, (5) are located the Muffle furnace calcination temperature and are set to 550 ℃, calcination time is 5 hours.Test obtain material modified through XRD, the powder body material that obtains is mainly anatase phase and rutile titanium dioxide.
Embodiment 9:
(1), (2), (3), (4) are with embodiment three, (5) are located the Muffle furnace calcination temperature and are set to 600 ℃, calcination time is 5 hours.Test obtain material modified through XRD, the powder body material that obtains is mainly anatase phase and rutile-type and deposits titanium dioxide.
Embodiment 10:
(1), (2), (3), (4) are with instance four, (5) are located the Muffle furnace calcination temperature and are set to 300 ℃, calcination time is 5 hours.Test obtain material modified through XRD, the powder body material that obtains is mainly anatase phase titanium dioxide.
Embodiment 11:
(1), (2), (3), (4) are with embodiment four, (5) are located the Muffle furnace calcination temperature and are set to 400 ℃, calcination time is 4 hours.Test obtain material modified through XRD, the powder body material that obtains is mainly anatase phase titanium dioxide.
Embodiment 12:
(1), (2), (3), (4) are with embodiment four, (5) are located the Muffle furnace calcination temperature and are set to 500 ℃, calcination time is 3 hours.Test obtain material modified through XRD, the powder body material that obtains is mainly anatase phase titanium dioxide.
Embodiment 13:
(1), (2), (3), (4) are with instance four, (5) are located the Muffle furnace calcination temperature and are set to 550 ℃, calcination time is 2 hours.Test obtain material modified through XRD, the powder body material that obtains is mainly anatase phase and rutile-type and deposits titanium dioxide.
Embodiment 14:
(1), (2), (3), (4) are with instance four, (5) are located the Muffle furnace calcination temperature and are set to 600 ℃, calcination time is 2 hours.Test obtain material modified through XRD, the powder body material that obtains is mainly anatase phase and rutile-type and deposits titanium dioxide.
Claims (10)
1. the preparation technology of an iron doped titanium dioxide powder is characterized in that, comprises following step:
(2), add hydrolysis inhibitor and obtain the homogeneous transparent solution A with adding absolute ethyl alcohol in the butyl titanate;
(2) mol ratio according to Ti and Fe is (20-5): 1, and with FeCl
36H
2O is dissolved in the absolute ethyl alcohol, forms FeCl
3Alcoholic solution B;
(3) at room temperature, solution B is joined in the solution A slowly stirred in the time of dropping, obtains the solution C of homogeneous transparent;
(4) solution C is stirred 15-30 minute after, leave standstill and carry out dried and obtain xerogel;
(5) xerogel is carried out heat treated and make the iron doped titanium dioxide powder.
2. preparation technology as claimed in claim 1 is characterized in that, the volume ratio of said butyl titanate and absolute ethyl alcohol is 1: 1-1: 2.
3. preparation technology as claimed in claim 1 is characterized in that said hydrolysis inhibitor is a glacial acetic acid, the volume ratio 10 of butyl titanate and glacial acetic acid: 1-10: 2.
4. preparation technology as claimed in claim 1; It is characterized in that said step (1) is specially: under the room temperature, under agitation slowly splash into butyl titanate in the beaker that fills ethanol; When stirring, slowly add glacial acetic acid, continue to stir the solution A that obtains homogeneous transparent.
5. preparation technology as claimed in claim 1 is characterized in that, the mass percent that the middle FeCl36H2O of said step (2) accounts for absolute ethyl alcohol is 3-15%.
6. preparation technology as claimed in claim 1 is characterized in that, the solution C time of repose is to leave standstill under the first room temperature 2 days in the said step (4), obtains yellow wet gel, places 48-72 hour naturally under the room temperature then.
7. preparation technology as claimed in claim 1 is characterized in that, dried is in the said step (4): solution C leaves standstill the back dries in temperature is set to 110-130 ℃ baking oven.
8. preparation technology as claimed in claim 1 is characterized in that, said step (5) is: xerogel is ground to form evengranular powder, be placed in the Muffle furnace calcination 2-5 hour, it is 200-700 ℃ that temperature is set.
9. preparation technology as claimed in claim 9 is characterized in that said calcination temperature is 200-500 ℃, and obtaining crystal formation is anatase sections doped titanium dioxide powder.
10. preparation technology as claimed in claim 9 is characterized in that said calcination temperature is 550-700 ℃, the iron doped titanium dioxide powder that obtains crystal formation and be rutile-type and Detitanium-ore-type and deposit.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102969168A (en) * | 2012-10-31 | 2013-03-13 | 彩虹集团公司 | Process for preparing doped titanium dioxide sol for dye-sensitized solar cell |
| CN103601238A (en) * | 2013-11-07 | 2014-02-26 | 昆明理工大学 | Method for preparing iron-doped TiO2 powder through microwave solid-phase reaction |
| CN103936294A (en) * | 2014-03-24 | 2014-07-23 | 同济大学 | Preparation method of coated glass sheet and photocatalytic water purifying device |
| CN103991902A (en) * | 2014-05-19 | 2014-08-20 | 中国矿业大学 | Preparation method of iron-doped anatase titanium dioxide microspheres with exposed surfaces {001} |
| CN104645963A (en) * | 2015-02-05 | 2015-05-27 | 昆明理工大学 | Method for inhibiting titanium dioxide phase change |
| CN105413689A (en) * | 2015-11-11 | 2016-03-23 | 中国科学院山西煤炭化学研究所 | Fe/TiO2 medium-temperature denitration catalyst and preparation method and application |
| CN105903486A (en) * | 2016-05-12 | 2016-08-31 | 深圳市尤佳环境科技有限公司 | Z-type photocatalyst and preparation method thereof |
| CN107134575A (en) * | 2017-03-30 | 2017-09-05 | 中南大学 | A kind of preparation method of anode material of lithium-ion battery |
| CN107556801A (en) * | 2017-08-23 | 2018-01-09 | 华南理工大学 | A kind of rust near-infrared high reflection material and preparation method thereof |
| CN108993506A (en) * | 2018-08-10 | 2018-12-14 | 张家港市汇鼎新材料科技有限公司 | A kind of preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite |
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| CN102969168A (en) * | 2012-10-31 | 2013-03-13 | 彩虹集团公司 | Process for preparing doped titanium dioxide sol for dye-sensitized solar cell |
| CN103601238A (en) * | 2013-11-07 | 2014-02-26 | 昆明理工大学 | Method for preparing iron-doped TiO2 powder through microwave solid-phase reaction |
| CN103601238B (en) * | 2013-11-07 | 2016-06-08 | 昆明理工大学 | A kind of microwave-assisted solid-state reaction method prepares the TiO of doping iron2The method of powder body |
| CN103936294B (en) * | 2014-03-24 | 2016-08-17 | 同济大学 | The preparation method of a kind of coated glass sheet and purifying device using photo-catalysis |
| CN103936294A (en) * | 2014-03-24 | 2014-07-23 | 同济大学 | Preparation method of coated glass sheet and photocatalytic water purifying device |
| CN103991902A (en) * | 2014-05-19 | 2014-08-20 | 中国矿业大学 | Preparation method of iron-doped anatase titanium dioxide microspheres with exposed surfaces {001} |
| CN103991902B (en) * | 2014-05-19 | 2015-04-22 | 中国矿业大学 | Preparation method of iron-doped anatase titanium dioxide microspheres with exposed surfaces {001} |
| CN104645963A (en) * | 2015-02-05 | 2015-05-27 | 昆明理工大学 | Method for inhibiting titanium dioxide phase change |
| CN105413689A (en) * | 2015-11-11 | 2016-03-23 | 中国科学院山西煤炭化学研究所 | Fe/TiO2 medium-temperature denitration catalyst and preparation method and application |
| CN105903486A (en) * | 2016-05-12 | 2016-08-31 | 深圳市尤佳环境科技有限公司 | Z-type photocatalyst and preparation method thereof |
| CN105903486B (en) * | 2016-05-12 | 2019-01-01 | 深圳市尤佳环境科技有限公司 | A kind of Z-type photochemical catalyst and preparation method thereof |
| CN107134575A (en) * | 2017-03-30 | 2017-09-05 | 中南大学 | A kind of preparation method of anode material of lithium-ion battery |
| CN107134575B (en) * | 2017-03-30 | 2020-05-15 | 中南大学 | Preparation method of sodium ion battery negative electrode material |
| CN107556801A (en) * | 2017-08-23 | 2018-01-09 | 华南理工大学 | A kind of rust near-infrared high reflection material and preparation method thereof |
| CN108993506A (en) * | 2018-08-10 | 2018-12-14 | 张家港市汇鼎新材料科技有限公司 | A kind of preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite |
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Application publication date: 20120718 |