CN104258850A - Ag-doped TiO2 nano thin film and composite material containing thin film - Google Patents
Ag-doped TiO2 nano thin film and composite material containing thin film Download PDFInfo
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- CN104258850A CN104258850A CN201410502474.6A CN201410502474A CN104258850A CN 104258850 A CN104258850 A CN 104258850A CN 201410502474 A CN201410502474 A CN 201410502474A CN 104258850 A CN104258850 A CN 104258850A
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Abstract
The invention discloses an Ag-doped TiO2 nano thin film and a composite material containing the thin film. The composite material is prepared by the following method: (1) mixing tetrabutyl titanate, absolute ethyl alcohol, nitric acid, acetyl acetone and deionized water, and fully stirring to obtain TiO2 sol; (2) adding AgNO3 into the TiO2 sol, and continuously stirring to obtain Ag-doped TiO2 sol; (3) preparing a wet film by a dip-lifting method by taking a special ceramic electrode material as a substrate; and (4) roasting in a muffle furnace to obtain the composite material consisting of the ceramic electrode material and a nano TiO2 coating layer, wherein a crystal phase formed on the ceramic electrode material is the Ag-doped TiO2 nano thin film. The Ag-doped TiO2 nano thin film disclosed by the invention is relatively high in catalysis activity. Through using the composite material, the degrading rate of benzene is increased by 26 percent when compared with the ceramic electrode material, and the degrading rate of benzene is over 80 percent.
Description
Technical field
The present invention relates to a kind of Ag doped Ti O with efficiently catalyzing and oxidizing effect
2nano thin-film, and the composite containing this film, belong to nano-TiO
2photocatalyst film manufactures field, applies to the manufacturing of the catalytic film material of low-temperature plasma catalyzing cooperation reactor.
Background technology
At present, along with the fast development of economy, various pernicious gas, such as VOC (VOCs), NOx, H
2s, SO
2deng discharge capacity also increasing sharply, the environment that the mankind depend on for existence in serious harm.The method of traditional process pernicious gas has combustion method, condensation method and absorption method etc.The low temperature plasma that development in recent years is got up and catalyst synergistic action technique, both the feature of non-thermal plasma trap convenient and efficient had been possessed, possesses again the high efficiency feature of catalytic oxidation pinpoint accuracy, therefore this technology possesses numerous advantage in process pernicious gas, has become the hot technology of process dusty gas.
The core of low-temperature plasma catalyzing cooperation technology is how to allow two kinds of technology combine organically and efficiently, and therefore preparation to be effectively combined with low-temperature plasma shedder and the good catalyst material of catalytic performance becomes the key studying and improve this technology.
TiO
2be light-catalysed catalyst the most frequently used at present, its catalytic effect is excellent.The technology of current making nano-titanium dioxide film is varied, such as vacuum vapor deposition method, chemical vapour deposition technique, sputtering method.Wang Dongliang etc. adopt vacuum vapor deposition method, load TiO on copper, glass plate, stainless steel 3 kinds of different materials
2film; Liu Peng etc. have studied with TiCl
4for titanium source, prepare TiO on a glass substrate by APCVD method (atmospheric chemical vapor method)
2the technique of film; Lin Zhidong etc. adopt magnetron sputtering method to prepare TiO
2nano thin-film.
Research shows, to TiO
2the structure of material and composition carry out modification and will effectively improve its catalytic effect to benzene, and method conventional at present has size to change method, transient metal doped method, semiconductors coupling method, noble metal loading method, sol gel method etc.Method of the present invention adopts sol-gal process and transient metal doped legal system for Ag doped Ti O
2nano film material.Sol-gal process is simple, and technological process is easy, convenient for industrialization large-scale production.The TiO of nano-scale
2possesses quantum size effect, the TiO when scantling is less than space charge layer
2photo-generated carrier directly migrate to semiconductor surface by simply spreading from inside particles, improve the quantum yield of reaction, thus photocatalysis performance significantly improved.The doping of transition metals Ag element, to TiO
2introduce impurity energy level, what form photo-generated carrier catches trap, extends the life-span of carrier thus improves photocatalysis usefulness.Ag doped Ti O is prepared by sol-gal process
2nano film material, not only method is simple, be convenient to be used in industry and change into product, and catalytic effect is good.
Summary of the invention
For above-mentioned prior art, for improving TiO
2the catalytic efficiency of film catalyst, the invention provides a kind of Ag doped Ti O
2nano thin-film, with and preparation method thereof, and the composite containing this film.
The present invention is achieved by the following technical solutions:
A kind of Ag doped Ti O
2the preparation method of nano thin-film, step is as follows:
(1) butyl titanate, absolute ethyl alcohol, nitric acid, acetylacetone,2,4-pentanedione and the deionized water proportioning according to volume ratio 7: 89.5: 0.5: 2: 1 is mixed, room temperature and 50% relative humidity condition under fully stir 1h, obtain TiO
2colloidal sol;
(2) TiO is accounted for according to doping metals Ag
2molar ratio be the ratio of 5%, to above-mentioned TiO
2the predecessor AgNO of doping metals is added in colloidal sol
3and Keep agitation 2h, seal ageing 24h afterwards, obtain the TiO of Ag doping
2colloidal sol;
(3) adopt special ceramic electrode material to be substrate, before film, ultrasonic 30min, then spends deionized water, then dries up with nitrogen; Then the TiO of the Ag doping of above-mentioned preparation is added
2colloidal sol, adopts the obtained wet film of dip-coating method (pull rate 5mm/s), natural drying 30min in air;
(4) in Muffle furnace with the ramp to 450 DEG C of 10 DEG C/min, roasting 2.5h, obtains ceramic electrode material and nano-TiO
2coat composed composite, the crystalline phase film that ceramic electrode material is formed is Ag doped Ti O
2nano thin-film.
Preferably, in described step (1), butyl titanate, absolute ethyl alcohol, nitric acid, acetylacetone,2,4-pentanedione are A.R. level.
Further, described butyl titanate can purchased from Solution on Chemical Reagents in Shanghai Co., Ltd.
In described step (3), special ceramic electrode material, has high apparent dielectric constant and lower dielectric absorption, prepares by the following method:
1. each raw material is taken by following mass percent: CaTiO
3, 68 ~ 75%; SrTiO
3, 15 ~ 20%; ZrO
2nano wire, 3 ~ 8%; BaTiO
3, 1.3%; TiO
2, 0.6%; ZnO, 1.4%; Bi
2o
3, 0.7%;
Each raw material is put into agate tank, is raw material in mass ratio: agate ball: absolute ethyl alcohol=1: the ratio of 2: 1 adds agate ball and ethanol, ball mill grinds 24h;
2. take out, dry, add polyvinyl alcohol (PVA) aqueous solution (submergence that mass fraction is 3%; For adhesive, for granulation), mixing, dries, granulation, crosses 200 mesh sieves;
3. internal diameter 0.6 ~ 1.0mm is depressed at 750kPa, external diameter 1.0 ~ 1.4mm, the capillary of length 30 ~ 60mm;
4. get above-mentioned capillary, in electric furnace, by intensification per hour 200 DEG C intensification, within one hour, carry out binder removal 800 DEG C of insulations, be then warming up to 1300 DEG C, heat preservation sintering 10 ~ 12 hours, slowly cools to room temperature, obtains ceramic capillary;
5. at ceramic capillary internal layer coating silver paste, sinter at 820 DEG C by silver (sintering 45 minutes), obtain the ZrO that adulterates
2the CaTiO of nano wire
3ceramic electrode material, is the special ceramic electrode material that the present invention is used.
Described ZrO
2nano wire is existing conventional products in prior art, the present invention ZrO used
2nano wire is purchased from Jinan flue thermal Ceramics Co., Ltd.
Preferably, described step 1. in, the proportion relation of each raw material is: CaTiO
3, 72%; SrTiO
3, 19%; ZrO
2nano wire, 5%; BaTiO
3, 1.3%; TiO
2, 0.6%; ZnO, 1.4%; Bi
2o
3, 0.7%.
Preferably, described step 2. in, PVA17-92 selected by polyvinyl alcohol.
Preferably, described step 3. in, be pressed into internal diameter 0.8mm, the capillary of external diameter 1.2mm, length 40mm.
Described silver paste is existing conventional products in prior art, is the Precious Metal of argentiferous, is be a kind of conductive material that dip-coating and silk screen process use the earliest in electronics industry.Consisting of of said method silver paste used: silver content is 70%, binder content is 15%, and organic carrier content is 15%; Described binding agent is the bismuth borosilicate glass of 8%; Each component by mass percentage.
TiO
2the catalytic effect of the size impact material of particle, the doping of transition metal also has larger impact to catalytic effect.Method of the present invention, uses sol-gal process on ceramic electrode material, prepare novel Ni doped Ti O
2nano film material nano-TiO
2, substantially increase its catalytic efficiency, may be used for process degraded pernicious gas, such as benzene.Ceramic electrode material of the present invention and nano-TiO
2coat composed composite, more only uses ceramic electrode material to improve about 26% to the degradation rate of benzene, reaches more than 80% to the degradation rate of benzene.
Accompanying drawing explanation
Fig. 1: benzene degradation rate contrast schematic diagram.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1 prepares Ag doped Ti O
2nano thin-film
Step is as follows:
(1) butyl titanate, absolute ethyl alcohol, nitric acid, acetylacetone,2,4-pentanedione and the deionized water proportioning according to volume ratio 7: 89.5: 0.5: 2: 1 is mixed (butyl titanate, absolute ethyl alcohol, nitric acid, acetylacetone,2,4-pentanedione being added successively in deionized water), room temperature and 50% relative humidity condition under fully stir 1h, obtain TiO
2colloidal sol;
(2) TiO is accounted for according to doping metals Ag
2molar ratio be the ratio of 5%, to above-mentioned TiO
2the predecessor AgNO of doping metals is added in colloidal sol
3and Keep agitation 2h, seal ageing 24h afterwards, obtain the TiO of Ag doping
2colloidal sol;
(3) adopt special ceramic electrode material to be substrate, before film, ultrasonic 30min, then spends deionized water, then dries up with nitrogen; Then the TiO of the Ag doping of above-mentioned preparation is added
2colloidal sol, adopts the obtained wet film of dip-coating method (pull rate 5mm/s), natural drying 30min in air;
(4) in Muffle furnace with the ramp to 450 DEG C of 10 DEG C/min, roasting 2.5h, obtains ceramic electrode material and nano-TiO
2coat composed composite, the crystalline phase film that ceramic electrode material is formed is Ag doped Ti O
2nano thin-film.
In described step (1), butyl titanate, absolute ethyl alcohol, nitric acid, acetylacetone,2,4-pentanedione are A.R. level.
Described butyl titanate is purchased from Solution on Chemical Reagents in Shanghai Co., Ltd.
In described step (3), special ceramic electrode material, prepares by the following method:
1. each raw material is taken by following mass percent: CaTiO
3, 72%; SrTiO
3, 19%; ZrO
2nano wire, 5%; BaTiO
3, 1.3%; TiO
2, 0.6%; ZnO, 1.4%; Bi
2o
3, 0.7%;
Each raw material is put into agate tank, is raw material in mass ratio: agate ball: absolute ethyl alcohol=1: the ratio of 2: 1 adds agate ball and ethanol, ball mill grinds 24h;
2. take out, dry, add polyvinyl alcohol (model PVA17-92) aqueous solution (submergence) that mass fraction is 3%, mixing, dry, granulation, cross 200 mesh sieves;
3. internal diameter 0.8mm is depressed at 750kPa, the capillary of external diameter 1.2mm, length 40mm;
4. get above-mentioned capillary, in electric furnace, by intensification per hour 200 DEG C intensification, within one hour, carry out binder removal 800 DEG C of insulations, be then warming up to 1300 DEG C, heat preservation sintering 11 hours, slowly cools to room temperature, obtains ceramic capillary;
5. at ceramic capillary internal layer coating silver paste, sinter at 820 DEG C by silver (sintering 45 minutes), namely obtain the ZrO that adulterates
2the CaTiO of nano wire
3ceramic electrode material, after testing, dielectric constant 82, dielectric loss (tan δ) is 0.0062, and fracture toughness is 6.2MPam
1/2.
Described ZrO
2nano wire is purchased from Jinan flue thermal Ceramics Co., Ltd.
Consisting of of described silver paste: silver content is 70%, binder content is 15%, and organic carrier content is 15%; Described binding agent is the bismuth borosilicate glass of 8%; Each component by mass percentage.
Test: for benzene, compares ceramic electrode material and nano-TiO prepared by the present embodiment
2coat composed composite, and ceramic electrode material (the special ceramic electrode material mentioned in the present embodiment) degradation rate to benzene.
Result is as shown in table 1 and Fig. 1.
The degradation rate statistical form unit of table 1 different materials degraded benzene: %
Time/min | Film+electronic ceramics | Electronic ceramics |
0 | 0 | 0 |
5 | 4 | 1 |
10 | 8 | 2 |
15 | 9 | 3 |
20 | 12 | 4 |
25 | 15 | 5 |
30 | 18 | 10 |
35 | 19 | 13 |
40 | 21 | 15 |
45 | 32 | 20 |
50 | 40 | 22 |
55 | 46 | 28 |
60 | 54 | 36 |
65 | 59 | 39 |
70 | 65 | 45 |
75 | 69 | 48 |
80 | 72 | 49 |
85 | 73 | 50 |
90 | 78 | 52 |
95 | 78 | 52 |
100 | 80 | 54 |
Conclusion: can be found out by table 1 and Fig. 1, composite of the present invention, to the degradation rate of benzene, after process 100min, reaches more than 80% to the degradation rate of benzene, more only uses ceramic electrode material to improve 26%.
Claims (10)
1. an Ag doped Ti O
2the preparation method of nano thin-film, is characterized in that: step is as follows:
(1) butyl titanate, absolute ethyl alcohol, nitric acid, acetylacetone,2,4-pentanedione and the deionized water proportioning according to volume ratio 7: 89.5: 0.5: 2: 1 is mixed, room temperature and 50% relative humidity condition under fully stir 1h, obtain TiO
2colloidal sol;
(2) TiO is accounted for according to doping metals Ag
2molar ratio be the ratio of 5%, to above-mentioned TiO
2the predecessor AgNO of doping metals is added in colloidal sol
3and Keep agitation 2h, seal ageing 24h afterwards, obtain the TiO of Ag doping
2colloidal sol;
(3) adopt special ceramic electrode material to be substrate, before film, ultrasonic 30min, then spends deionized water, then dries up with nitrogen; Then the TiO of the Ag doping of above-mentioned preparation is added
2colloidal sol, adopts dip-coating method to obtain wet film, natural drying 30min in air;
(4) in Muffle furnace with the ramp to 450 DEG C of 10 DEG C/min, roasting 2.5h, ceramic electrode material is formed crystalline phase film, is Ag doped Ti O
2nano thin-film.
2. a ceramic electrode material and nano-TiO
2the preparation method of coat composed composite, it is characterized in that: step is as follows: butyl titanate, absolute ethyl alcohol, nitric acid, acetylacetone,2,4-pentanedione and the deionized water proportioning according to a definite sequence and volume ratio 7: 89.5: 0.5: 2: 1 mixes by (1), room temperature and 50% relative humidity condition under fully stir 1h, obtain TiO
2colloidal sol;
(2) TiO is accounted for according to doping metals Ag
2molar ratio be the ratio of 5%, to above-mentioned TiO
2the predecessor AgNO of doping metals is added in colloidal sol
3and Keep agitation 2h, seal ageing 24h afterwards, obtain the TiO of Ag doping
2colloidal sol;
(3) adopt special ceramic electrode material to be substrate, before film, ultrasonic 30min, then spends deionized water, then dries up with nitrogen; Then the TiO of the Ag doping of above-mentioned preparation is added
2colloidal sol, adopts dip-coating method to obtain wet film, natural drying 30min in air;
(4) in Muffle furnace with the ramp to 450 DEG C of 10 DEG C/min, roasting 2.5h, obtains ceramic electrode material and nano-TiO
2coat composed composite.
3. preparation method according to claim 1 and 2, is characterized in that: in described step (3), special ceramic electrode material, prepares by the following method:
1. each raw material is taken by following mass percent: CaTiO
3, 68 ~ 75%; SrTiO
3, 15 ~ 20%; ZrO
2nano wire, 3 ~ 8%; BaTiO
3, 1.3%; TiO
2, 0.6%; ZnO, 1.4%; Bi
2o
3, 0.7%;
Each raw material is put into agate tank, is raw material in mass ratio: agate ball: absolute ethyl alcohol=1: the ratio of 2: 1 adds agate ball and ethanol, ball mill grinds 24h;
2. take out, dry, add the polyvinyl alcohol water solution that mass fraction is 3%, mixing, dry, granulation, cross 200 mesh sieves;
3. internal diameter 0.6 ~ 1.0mm is depressed at 750kPa, external diameter 1.0 ~ 1.4mm, the capillary of length 30 ~ 60mm;
4. get above-mentioned capillary, in electric furnace, by intensification per hour 200 DEG C intensification, within one hour, carry out binder removal 800 DEG C of insulations, be then warming up to 1300 DEG C, heat preservation sintering 10 ~ 12 hours, slowly cools to room temperature, obtains ceramic capillary;
5. at ceramic capillary internal layer coating silver paste, sinter silver-colored at 820 DEG C, obtain mixing ceramic electrode material.
4. preparation method according to claim 3, is characterized in that: described step 1. in, the proportion relation of each raw material is: CaTiO
3, 72%; SrTiO
3, 19%; ZrO
2nano wire, 5%; BaTiO
3, 1.3%; TiO
2, 0.6%; ZnO, 1.4%; Bi
2o
3, 0.7%.
5. preparation method according to claim 3, is characterized in that: described step 2. in, PVA17-92 selected by polyvinyl alcohol.
6. preparation method according to claim 3, is characterized in that: described step 3. in, be pressed into internal diameter 0.8mm, the capillary of external diameter 1.2mm, length 40mm.
7. utilize the preparation-obtained Ag doped Ti O of the preparation method according to any one of claim 1 ~ 6
2nano thin-film.
8. Ag doped Ti O according to claim 7
2the application of nano thin-film in degraded pernicious gas.
9. utilize the preparation-obtained ceramic electrode material of the preparation method according to any one of claim 1 ~ 6 and nano-TiO
2coat composed composite.
10. the application of composite according to claim 9 in degraded pernicious gas.
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Cited By (8)
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CN105289571A (en) * | 2015-11-02 | 2016-02-03 | 卢俊清 | La-doped TiO2 nano-catalysis material used for low-temperature plasma catalysis synergistic effect |
CN108620007A (en) * | 2018-03-30 | 2018-10-09 | 华南农业大学 | A kind of electrical enhanced photocatalysis reaction unit and its application based on fruit freshness preserving |
CN109012667A (en) * | 2018-08-07 | 2018-12-18 | 景德镇陶瓷大学 | A kind of highlight catalytic active Ag doping CaTi2O5The preparation method of nano material and its product obtained |
CN109411599A (en) * | 2018-10-22 | 2019-03-01 | 西安理工大学 | A kind of preparation method of zirconium adulterated TiOx memristor film |
CN109876805A (en) * | 2017-12-06 | 2019-06-14 | 天津发洋环保科技有限公司 | A kind of Ag doping TiO2The preparation method of nano photo-catalytic |
CN111774056A (en) * | 2020-06-23 | 2020-10-16 | 西安航空职业技术学院 | Preparation method of silver-modified titanium dioxide-calcium titanate crystal thin film material |
CN113429222A (en) * | 2021-07-16 | 2021-09-24 | 重庆大学 | Ag/TiO2Photocatalytic ceramic tile and preparation method thereof |
WO2022222996A1 (en) * | 2021-04-23 | 2022-10-27 | 李彦军 | Nano-titanate, nano-titanic acid, and nano-tio2 containing doping ag, preparation method therefor and use thereof |
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CN105289571A (en) * | 2015-11-02 | 2016-02-03 | 卢俊清 | La-doped TiO2 nano-catalysis material used for low-temperature plasma catalysis synergistic effect |
CN109876805A (en) * | 2017-12-06 | 2019-06-14 | 天津发洋环保科技有限公司 | A kind of Ag doping TiO2The preparation method of nano photo-catalytic |
CN108620007A (en) * | 2018-03-30 | 2018-10-09 | 华南农业大学 | A kind of electrical enhanced photocatalysis reaction unit and its application based on fruit freshness preserving |
CN109012667A (en) * | 2018-08-07 | 2018-12-18 | 景德镇陶瓷大学 | A kind of highlight catalytic active Ag doping CaTi2O5The preparation method of nano material and its product obtained |
CN109012667B (en) * | 2018-08-07 | 2021-07-20 | 景德镇陶瓷大学 | Ag-doped CaTi with high photocatalytic activity2O5Preparation method of nano material and product prepared by preparation method |
CN109411599A (en) * | 2018-10-22 | 2019-03-01 | 西安理工大学 | A kind of preparation method of zirconium adulterated TiOx memristor film |
CN111774056A (en) * | 2020-06-23 | 2020-10-16 | 西安航空职业技术学院 | Preparation method of silver-modified titanium dioxide-calcium titanate crystal thin film material |
CN111774056B (en) * | 2020-06-23 | 2022-12-27 | 西安航空职业技术学院 | Preparation method of silver-modified titanium dioxide-calcium titanate crystal thin film material |
WO2022222996A1 (en) * | 2021-04-23 | 2022-10-27 | 李彦军 | Nano-titanate, nano-titanic acid, and nano-tio2 containing doping ag, preparation method therefor and use thereof |
CN113429222A (en) * | 2021-07-16 | 2021-09-24 | 重庆大学 | Ag/TiO2Photocatalytic ceramic tile and preparation method thereof |
CN113429222B (en) * | 2021-07-16 | 2023-02-21 | 重庆大学 | Ag/TiO material 2 Photocatalytic ceramic tile and preparation method thereof |
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