CN104028256A - Method for preparing porous TiO2 film - Google Patents
Method for preparing porous TiO2 film Download PDFInfo
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- CN104028256A CN104028256A CN201410243216.0A CN201410243216A CN104028256A CN 104028256 A CN104028256 A CN 104028256A CN 201410243216 A CN201410243216 A CN 201410243216A CN 104028256 A CN104028256 A CN 104028256A
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Abstract
The invention provides a method for preparing a porous TiO2 film. The method comprises the following steps: spinning a substrate with TiO2 slurry by using a uniform gel heating machine in the speed of 1800-2500r/s; drying for 0.5-1 hour at 60-80 DEG C; subsequently performing thermal treatment on the dried film layer, wherein in the thermal treatment, the annealing temperature is 420-550 DEG C, and the annealing time is 0.5-1 hours, so that the TiO2 film is obtained; the TiO2 slurry is prepared by grinding nano TiO2 powder and anhydrous acetic acid, subsequently adding deionized water and absolute ethyl alcohol, grinding respectively, and finally dropping an ethyl cellulose solution and terpilenol. The porous TiO2 film prepared by using the method is excellent in uniformity and compactness, relatively high in adhesion property with a glass substrate, good in long-lasting stability of the slurry, free of phenomena such as layering or agglomeration, simple in preparation method, low in cost and applicable to on-scale production.
Description
Technical field
The present invention relates to technical field of coatings, be specifically related to a kind of porous TiO
2the preparation method of film.
Background technology
In recent years, because photochemical catalyst has potential using value in every field, researcher is paying huge effort aspect Development of Novel photochemical catalyst.Consider the factor of each side, TiO
2because it is inexpensive, nontoxic, good stability and catalytic efficiency high, become the photochemical catalyst that has application prospect most.But due to nanoscale TiO
2little, the specific area of particle diameter and surface can be all very large, and coordination wretched insufficiency, shows extremely strong surface polarity, and its powder is easily reunited in water, particularly in organic solvent, is also difficult for disperseing, and Powdered TiO
2be difficult to separate and reclaim and easily loss.Therefore, research TiO
2the dispersion of powder, to be easy to reclaim be prerequisite and the basis of further improving its photocatalytic applications performance.
In recent years, in order to improve nano-TiO
2the dispersiveness of powder in solvent, different processing methods is studied mistake, and wherein the most general method is to add to stir by grinding to be prepared into TiO
2water paste.But it is by direct dispersant and nano-TiO that traditional grinding adds paddling process
2powder grinds and stirs, and the slurry obtaining is easily reunited, and water paste easily cracks in blade coating process and preparation condition is not easy to control.
Existing TiO
2film is mainly prepared gained by spread coating, spraying process, dip coating or knife coating, but these methods need to rely on operating personnel's skills involved in the labour in the preparation, the uniformity of its film is difficult to ensure card, and the method equipment needed thereby and the instrument that have are expensive, condition harshness, complicated operation.
Summary of the invention
The object of the present invention is to provide a kind of porous TiO
2the preparation method of film, makes the film of system have higher uniformity.
Technical scheme of the present invention is as follows: a kind of porous TiO
2the preparation method of film with the roasting glue machine of even glue under the speed of 1800-2500r/s by TiO
2slurry for rotary coating to substrate, and at 60-80 DEG C drying and processing 0.5-1h; Then the rete after drying is heat-treated, its heat treated annealing temperature be 420-550 DEG C, annealing time be 0.5-1 hour porous TiO
2film; Described TiO
2slurry makes according to following preparation method:
(1) by nano-TiO
2powder and anhydrous acetic acid are put into ceramic mortar and are ground 2-8min, TiO
2with the mass volume ratio of anhydrous acetic acid be 1: 0.5 ~ 2 g/ml;
(2) in (1), add deionized water to grind 1-6min, and repeat this operation 3-10 time, described TiO
2with the mass volume ratio of the each addition of deionized water be 1:0.5 ~ 2g/ml;
(3) in (2), add absolute ethyl alcohol to grind 1-6min, and repeat this operation 8-20 time, described TiO
2with the mass volume ratio of the each addition of absolute ethyl alcohol be 1:0.5 ~ 2g/ml;
(4) in (3), add absolute ethyl alcohol to grind 1-6min, and repeat this operation 3-10 time, described TiO
2with the mass volume ratio of the each addition of absolute ethyl alcohol be 1:2 ~ 4g/ml;
(5) will grind the TiO making through (4)
2slurry is transferred in beaker, and under strong magnetic agitation, ethyl cellulose solution and terpinol is dropwise joined to TiO successively
2in slurry, after being added dropwise to complete, continue again to stir 1-5min; The wherein addition of ethyl cellulose and TiO
2mass ratio be 0.3: 1 ~ 2.5: 1, the addition of terpinol and TiO
2mass ratio be 0.25: 1 ~ 2: 1;
(6) slurry (5) being made leaves standstill 10-30s in Ultrasound Instrument after ultrasonic processing 10-30s, then it is stirred to 1-5min under strong magnetic agitation; Then repeat above-mentioned ultrasonic, leave standstill and whipping step 2-8 time;
(7) by through (6) stir slurry under 40-70 DEG C of condition, continues stir be concentrated into slurry in contain TiO
2mass percent be 3-20%, obtain TiO
2slurry.
Further, described substrate refers to after, deionized water ultrasonic cleaning 3-7min clean through washing powder rinsing the slide of drying and processing again.
Described strong magnetic agitation refers to and stirs with the magnetic apparatus that rotating speed is 300-600rpm.
Nano-TiO in described step (1)
2powder is that particle diameter is the pure sharp titanium nano titanium oxide of 12-18nm.
Ethyl cellulose solution in described step (5) is under 40 DEG C of constant temperature stirring conditions, and ethyl cellulose is slowly dissolved in and is obtained in absolute ethyl alcohol according to the mass ratio of 1: 12; Ethyoxyl mass content in described ethyl cellulose is 47.5%-49.0%.
Be that the present invention is taking business nano TiO 2 powder as raw material and taking absolute ethyl alcohol as dispersant, and using ethyl cellulose simultaneously as binding agent and pore creating material, be prepared into slurry by polishing progressively, make nano-TiO
2particle is uniformly dispersed, and makes the TiO making
2slurry do not reunite, not stratified, dispersed, good stability.Then by spin-coating and high annealing method, by the TiO making
2slurry is prepared even, fine and close porous TiO on substrate
2rete.
With respect to prior art, the present invention has following beneficial effect:
1, porous TiO of the present invention
2film adopts TiO
2slurry is rotated prepared by coating method, the film making has even, the fine and close feature of film, and in film, only contain two kinds of polymer substances, not only preparation process is easy, with low cost, and also easily remove by high annealing the polymer substance containing in film, thereby obtain porous TiO
2film.
2, the present invention adopts progressively polishing first to use anhydrous acetic acid and deionized water to TiO
2powder carries out pretreatment, be then slowly scattered in absolute ethyl alcohol, then add wherein ethyl cellulose solution and terpinol, the slurry of preparing not to reunite, not stratified and dispersed, stability is all good.
3, need to add the multiple polymer substances such as dispersant, emulsifying agent, pore creating material, powder covering with respect to traditional slurry preparation process, the present invention only need to add these two kinds of polymer substances of ethyl cellulose and terpinol, and simple to operate, be easy to realize, and repeatability is high.
4, the ethyl cellulose in the present invention is binding agent, is again pore creating material; Terpinol is levelling agent, reduces the interpolation of auxiliary agent, improves dispersiveness and the stability of slurry.
Brief description of the drawings
Fig. 1 is TiO
2film Electronic Speculum figure, wherein a is TiO prepared by the embodiment of the present invention 3
2film Electronic Speculum figure; B is TiO prepared by comparative example 1
2film Electronic Speculum figure; C is TiO prepared by comparative example 2
2film Electronic Speculum figure;
Fig. 2 is TiO prepared by the embodiment of the present invention 1
2film amplifies the field emission scanning electron microscope figure of 2,000 times, and wherein d is TiO
2electronic Speculum figure before film calcination, e is TiO
2electronic Speculum figure after film calcining;
Fig. 3 is TiO prepared by the embodiment of the present invention 1
2film amplifies the field emission scanning electron microscope figure of 10,000 times, and wherein f is TiO
2electronic Speculum figure before film calcination, g is TiO
2electronic Speculum figure after film calcining;
Fig. 4 is TiO prepared by the embodiment of the present invention 2
2film is the light degradation curve to methylene blue under natural daylight, and wherein h is TiO
2light degradation curve before film calcination, i is TiO
2light degradation curve after film calcination.
Detailed description of the invention
The nano-TiO adopting in embodiment below
2powder is that to select particle diameter be the pure sharp titanium nano titanium oxide of 15nm;
Strong magnetic agitation refers to and stirs with the magnetic apparatus that rotating speed is 300-600rpm;
Selected ethyl cellulose solution is that ethyl cellulose is slowly dissolved in absolute ethyl alcohol and is obtained according to the mass ratio of 1: 12, and wherein the ethyoxyl mass content in ethyl cellulose is 47.5%-49.0%.
Embodiment 1:
(1) by nanometer 3g TiO
2powder and 3ml anhydrous acetic acid are put into ceramic mortar and are ground 8min;
(2) in (1), add 3ml deionized water to grind 6min, and repeat this operation 5 times;
(3) in (2), add 3ml absolute ethyl alcohol to grind 6min, and repeat this operation 15 times;
(4) in (3), add 6ml absolute ethyl alcohol to grind 6min, and repeat this operation 5 times;
(5) will grind the TiO making through (4)
2slurry is transferred in beaker, under strong magnetic agitation, 1.5g ethyl cellulose solution and 0.9g terpinol is dropwise joined to TiO successively
2in slurry, after being added dropwise to complete, continue again to stir 1min;
(6) slurry (5) being made leaves standstill 10s in Ultrasound Instrument after ultrasonic processing 10s, then it is stirred to 1min under strong magnetic agitation; Then repeat above-mentioned ultrasonic, leave standstill and whipping step 6 times;
(7) by through (6) stir slurry under 50 DEG C of conditions, continues stir be concentrated into slurry in contain TiO
2mass percent be 20%, obtain TiO
2slurry.
(8) substrate: by drying and processing again after clean through washing powder rinsing slide, deionized water ultrasonic cleaning 5min;
(9) with the roasting glue machine of even glue under the speed of 2000r/s by the TiO making
2slurry for rotary coating to treated substrate, and at 60 DEG C drying and processing 1h;
(10) rete after drying is heat-treated to obtain to porous TiO
2film, its heat treated annealing temperature is that 420 DEG C, annealing time are 1 hour.
Porous TiO prepared by the present embodiment
2as shown in Figure 2, in Fig. 2, d is the Electronic Speculum figure before calcination to the field emission scanning electron microscope figure that film amplification is 2,000 times, and e is the Electronic Speculum figure after calcining, from scheming, and porous TiO prepared by the present invention
2film is very even, fine and close, and film after calcining is still very even and fine and close, and presents loose structure.Amplify the field emission scanning electron microscope figure of 10,000 times as shown in Figure 3, in Fig. 3, f is the Electronic Speculum figure before calcination, and g is the Electronic Speculum figure after calcining, and before and after its calcining, the pattern of film is similar.
Embodiment 2:
(1) by nanometer 1.5g TiO
2powder and 3ml anhydrous acetic acid are put into ceramic mortar and are ground 3min;
(2) in (1), add 3ml deionized water to grind 2min, and repeat this operation 3 times;
(3) in (2), add 3ml absolute ethyl alcohol to grind 2min, and repeat this operation 10 times;
(4) in (3), add 6ml absolute ethyl alcohol to grind 5min, and repeat this operation 4 times;
(5) will grind the TiO making through (4)
2slurry is transferred in beaker, under strong magnetic agitation, 1g ethyl cellulose solution and 1g terpinol is dropwise joined to TiO successively
2in slurry, after being added dropwise to complete, continue again to stir 2min;
(6) slurry (5) being made leaves standstill 20s in Ultrasound Instrument after ultrasonic processing 20s, then it is stirred to 2min under strong magnetic agitation; Then repeat above-mentioned ultrasonic, leave standstill and whipping step 5 times;
(7) by through (6) stir slurry under 45 DEG C of conditions, continues stir be concentrated into slurry in contain TiO
2mass percent be 15%, obtain TiO
2slurry.
(8) substrate: by drying and processing again after clean through washing powder rinsing slide, deionized water ultrasonic cleaning 7min;
(9) with the roasting glue machine of even glue under the speed of 1800r/s by TiO
2slurry for rotary coating is on substrate, and at 80 DEG C drying and processing 0.5h;
(10) rete after drying is heat-treated to obtain to porous TiO
2film, its heat treated annealing temperature is that 450 DEG C, annealing time are 1 hour.
Porous TiO prepared by the present embodiment
2film is forward and backward to the light degradation curve of methylene blue h, i as shown in Figure 4 in calcination, the porous TiO obtaining from the known calcining of two curves
2the light degradation successful of film is better than the TiO before calcining
2film.
Embodiment 3:
(1) by nanometer 1g TiO
2powder and 1ml anhydrous acetic acid are put into ceramic mortar and are ground 2min;
(2) in (1), add 1ml deionized water to grind 2min, and repeat this operation 3 times;
(3) in (2), add 1ml absolute ethyl alcohol to grind 1min, and repeat this operation 8 times;
(4) in (3), add 2ml absolute ethyl alcohol to grind 1min, and repeat this operation 5 times;
(5) will grind the TiO making through (4)
2slurry is transferred in beaker, under strong magnetic agitation, 0.5g ethyl cellulose solution and 0.5g terpinol is dropwise joined to TiO successively
2in slurry, after being added dropwise to complete, continue again to stir 1min;
(6) slurry (5) being made leaves standstill 15s in Ultrasound Instrument after ultrasonic processing 15s, then it is stirred to 1min under strong magnetic agitation; Then repeat above-mentioned ultrasonic, leave standstill and whipping step 3 times;
(7) by through (6) stir slurry under 50 DEG C of conditions, continues stir be concentrated into slurry in contain TiO
2mass percent be 10%, obtain TiO
2slurry.
(8) substrate; By drying and processing again after clean through washing powder rinsing slide, deionized water ultrasonic cleaning 3min;
(9) with the roasting glue machine of even glue under the speed of 2500r/s by TiO
2slurry for rotary coating is on substrate, and at 70 DEG C drying and processing 1h;
(10) rete after drying is heat-treated to obtain to porous TiO
2film, its heat treated annealing temperature is that 550 DEG C, annealing time are 0.8 hour.
Embodiment 4:
(1) by nanometer 2g TiO
2powder and 1ml anhydrous acetic acid are put into ceramic mortar and are ground 5min;
(2) in (1), add 2ml deionized water to grind 3min, and repeat this operation 7 times;
(3) in (2), add 2ml absolute ethyl alcohol to grind 2min, and repeat this operation 12 times;
(4) in (3), add 4ml absolute ethyl alcohol to grind 2min, and repeat this operation 8 times;
(5) will grind the TiO making through (4)
2slurry is transferred in beaker, under strong magnetic agitation, 2g ethyl cellulose solution and 1.2g terpinol is dropwise joined to TiO successively
2in slurry, after being added dropwise to complete, continue again to stir 3min;
(6) slurry (5) being made leaves standstill 25s in Ultrasound Instrument after ultrasonic processing 25s, then it is stirred to 1min under strong magnetic agitation; Then repeat above-mentioned ultrasonic, leave standstill and whipping step 6 times;
(7) by through (6) stir slurry under 70 DEG C of conditions, continues stir be concentrated into slurry in contain TiO
2mass percent be 3%, obtain TiO
2slurry.
(8) substrate: by after clean through washing powder rinsing slide, deionized water ultrasonic cleaning 5min again drying and processing obtain.
(9) with the roasting glue machine of even glue under the speed of 2000r/s by TiO
2slurry for rotary coating is on substrate, and at 80 DEG C drying and processing 0.5h;
(10) rete after drying is heat-treated to obtain to porous TiO
2film, its heat treated annealing temperature is that 550 DEG C, annealing time are 0.5 hour.
Comparative example 1:
(1) by nanometer 1g TiO
2powder and 1ml anhydrous acetic acid are put into ceramic mortar and are ground 2min;
(2) in (1), add 1ml deionized water to grind 2min, and repeat this operation 3 times;
(3) in (2), add 1ml absolute ethyl alcohol to grind 1min, and repeat this operation 8 times;
(4) in (3), add 2ml absolute ethyl alcohol to grind 1min, and repeat this operation 5 times;
(5) will grind the TiO making through (4)
2slurry is transferred in beaker, under strong magnetic agitation, 0.5g ethyl cellulose solution, 0.5g terpinol and 0.5g polyethylene glycol is joined to TiO successively
2in slurry, after being added dropwise to complete, continue again to stir 1min;
(6) slurry (5) being made leaves standstill 15s in Ultrasound Instrument after ultrasonic processing 15s, then it is stirred to 1min under strong magnetic agitation; Then repeat above-mentioned ultrasonic, leave standstill and whipping step 3 times;
(7) by through (6) stir slurry under 50 DEG C of conditions, continues stir be concentrated into slurry in contain TiO
2mass percent be 10%, obtain TiO
2slurry.
(8) substrate; By drying and processing again after clean through washing powder rinsing slide, deionized water ultrasonic cleaning 3min;
(9) with the roasting glue machine of even glue under the speed of 2500r/s by TiO
2slurry for rotary coating is on substrate, and at 70 DEG C drying and processing 1h.
Comparative example 2:
(1) P25 powder was carried out to acid treatment before test, adopt aqueous solution of nitric acid, acidity is controlled at PH=2, and temperature is processed 10 hours in the waters of 80 DEG C, handles later P25 dry for standby in the baking oven of 85 DEG C;
(2) take the P25 block 3g after acid treatment, mix in mortar with OP emulsifying agent, polyethylene glycol, water, the ratio of P25 block, OP emulsifying agent, PEG, water is 3: 0.5: 0.5: 3, make P25 block preliminarily solubilised;
(3) solution obtaining is stirred 1.5 hours under the condition of 50 DEG C, then be warmed up to 80 DEG C of stirrings 2 hours;
(4) under 80 DEG C of conditions, stir concentrated above-mentioned slurry to the proportion of titanium dioxide and account for 15%, obtain titania slurry;
(5) substrate; By drying and processing again after clean through washing powder rinsing slide, deionized water ultrasonic cleaning 3min;
(6) with the roasting glue machine of even glue under the speed of 2500r/s by TiO
2slurry for rotary coating is on substrate, and at 70 DEG C drying and processing 1h.
Porous TiO prepared by embodiment 3
2the Electronic Speculum figure of the film that film is prepared with comparative example 1-2 contrasts as shown in Figure 1, and wherein a is TiO prepared by the embodiment of the present invention 3
2film Electronic Speculum figure; B is TiO prepared by comparative example 1
2film Electronic Speculum figure; C is TiO prepared by comparative example 2
2film Electronic Speculum figure; Relatively a, b and c are known, and the present invention prepares TiO
2film forming, uniformity and the compactness of slurry all will be got well compared with the slurry of configuration in comparative example 1,2; And the present invention adds only two kinds of materials, this technology is simple, Yi Hang.
Above embodiment is not limited only to protection scope of the present invention, all modify based on basic thought of the present invention or change all belong to protection scope of the present invention.
Claims (5)
1. a porous TiO
2the preparation method of film, is characterized in that: with the roasting glue machine of even glue under the speed of 1800-2500r/s by TiO
2slurry for rotary coating to substrate, and at 60-80 DEG C drying and processing 0.5-1h; Then the rete after drying is heat-treated, its heat treated annealing temperature be 420-550 DEG C, annealing time be 0.5-1 hour porous TiO
2film;
Described TiO
2slurry is to make according to following preparation method:
(1) by nano-TiO
2powder and anhydrous acetic acid are put into ceramic mortar and are ground 2-8min, TiO
2with the mass volume ratio of anhydrous acetic acid be 1: 0.5 ~ 2 g/ml;
(2) in (1), add deionized water to grind 1-6min, and repeat this operation 3-10 time, described TiO
2with the mass volume ratio of the each addition of deionized water be 1:0.5 ~ 2g/ml;
(3) in (2), add absolute ethyl alcohol to grind 1-6min, and repeat this operation 8-20 time, described TiO
2with the mass volume ratio of the each addition of absolute ethyl alcohol be 1:0.5 ~ 2g/ml;
(4) in (3), add absolute ethyl alcohol to grind 1-6min, and repeat this operation 3-10 time, described TiO
2with the mass volume ratio of the each addition of absolute ethyl alcohol be 1:2 ~ 4g/ml;
(5) will grind the TiO making through (4)
2slurry is transferred in beaker, and under strong magnetic agitation, ethyl cellulose solution and terpinol is dropwise joined to TiO successively
2in slurry, after being added dropwise to complete, continue again to stir 1-5min; The wherein addition of ethyl cellulose and TiO
2mass ratio be 0.3: 1 ~ 2.5: 1, the addition of terpinol and TiO
2mass ratio be 0.25: 1 ~ 2: 1;
(6) slurry (5) being made leaves standstill 10-30s in Ultrasound Instrument after ultrasonic processing 10-30s, then it is stirred to 1-5min under strong magnetic agitation; Then repeat above-mentioned ultrasonic, leave standstill and whipping step 2-8 time;
(7) by through (6) stir slurry under 40-70 DEG C of condition, continues stir be concentrated into slurry in contain TiO
2mass percent be 3-20%, obtain TiO
2slurry.
2. TiO according to claim 1
2the preparation method of slurry, is characterized in that: described substrate refers to after, deionized water ultrasonic cleaning 3-7min clean through washing powder rinsing the slide of drying and processing again.
3. porous TiO according to claim 1
2method for manufacturing thin film, is characterized in that: described strong magnetic agitation refers to and stirs with the magnetic apparatus that rotating speed is 300-600rpm.
4. porous TiO according to claim 1
2method for manufacturing thin film, is characterized in that: the nano-TiO in described step (1)
2powder is that particle diameter is the pure sharp titanium nano titanium oxide of 12-18nm.
5. porous TiO according to claim 1
2method for manufacturing thin film, is characterized in that: the ethyl cellulose solution in described step (5) is under 40 DEG C of constant temperature stirring conditions, and ethyl cellulose is slowly dissolved in and is obtained in absolute ethyl alcohol according to the mass ratio of 1: 12; Ethyoxyl mass content in described ethyl cellulose is 47.5%-49.0%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109046302A (en) * | 2018-08-27 | 2018-12-21 | 合肥工业大学 | A kind of porous petal-like anatase TiO2Nano-crystal film and preparation method thereof |
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