CN104028256B - A kind of porous TiO 2the preparation method of film - Google Patents
A kind of porous TiO 2the preparation method of film Download PDFInfo
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- CN104028256B CN104028256B CN201410243216.0A CN201410243216A CN104028256B CN 104028256 B CN104028256 B CN 104028256B CN 201410243216 A CN201410243216 A CN 201410243216A CN 104028256 B CN104028256 B CN 104028256B
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Abstract
The invention provides a kind of porous TiO
2the preparation method of film, bakes glue machine under the speed of 1800-2500r/min by TiO with even glue
2slurry for rotary coating on substrate, and at 60-80 DEG C drying and processing 0.5-1h; Then by dry after rete heat-treat, its heat treated annealing temperature is 420-550 DEG C, annealing time be 0.5-1 hour porous TiO
2film; Described TiO
2slurry is by nano-TiO
2powder and anhydrous acetic acid grind, and then add deionized water and absolute ethyl alcohol grinds respectively, are finally added dropwise to ethyl cellulose solution and terpinol and obtain.Porous TiO prepared by the present invention
2film has excellent uniformity and compactness and higher and slurry long-time stability are good with the adhesive force of glass substrate, do not occur the phenomenon of layering and reunion, and preparation method is simple, with low cost, is suitable for large-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 has paid huge effort in 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 having application prospect most.But due to nanoscale TiO
2little, the specific area of particle diameter and surface energy all very large, and coordination wretched insufficiency, shows extremely strong surface polarity, its powder is easily reunited in water, particularly also not easily disperses in organic solvent, and Powdered TiO
2be difficult to separation and recovery and easily run off.Therefore, TiO is studied
2the dispersion of powder, to be easy to reclaim be prerequisite and the basis of improving its photocatalytic applications performance further.
In recent years, in order to improve nano-TiO
2powder dispersiveness in a solvent, different processing methods is studied mistake, and wherein the most general method adds to stir by grinding to be prepared into TiO
2water paste.But it is that dispersant is direct and nano-TiO that traditional grinding adds paddling process
2powder carries out grinding and stirring, and the slurry obtained easily is reunited, and water paste easily crack in knifing process and preparation condition be not easy control.
Existing TiO
2film mainly prepares gained by spread coating, spraying process, dip coating or knife coating, but these methods need the skills involved in the labour relying on operating personnel in the preparation, the uniformity of its film is comparatively difficult to ensure card, and the method equipment needed thereby had and instrument price are expensive, condition is harsh, 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 bakes glue machine under the speed of 1800-2500r/min by TiO with even glue
2slurry for rotary coating on substrate, and at 60-80 DEG C drying and processing 0.5-1h; Then by dry after rete heat-treat, its heat treated annealing temperature is 420-550 DEG C, annealing time be 0.5-1 hour porous TiO
2film; Described TiO
2slurry obtains 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
2be 1:0.5 ~ 2g/ml with the mass volume ratio of anhydrous acetic acid;
(2) in (1), add deionized water and carry out grinding 1-6min, and repeat this operation 3-10 time, described TiO
2be 1:0.5 ~ 2g/ml with the mass volume ratio of each addition of deionized water;
(3) in (2), add absolute ethyl alcohol and carry out grinding 1-6min, and repeat this operation 8-20 time, described TiO
2be 1:0.5 ~ 2g/ml with the mass volume ratio of each addition of absolute ethyl alcohol;
(4) in (3), add absolute ethyl alcohol and carry out grinding 1-6min, and repeat this operation 3-10 time, described TiO
2be 1:2 ~ 4g/ml with the mass volume ratio of each addition of absolute ethyl alcohol;
(5) TiO that will obtain through (4) grinding
2slurry is transferred in beaker, and under strong magnetic agitation, ethyl cellulose solution and terpinol is dropwise joined TiO successively
2in slurry, continue again after being added dropwise to complete 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 obtained to (5) is left standstill 10-30s after ultrasonic process 10-30s in Ultrasound Instrument, then it is stirred 1-5min under strong magnetic agitation; Then repeat above-mentioned ultrasonic, leave standstill and whipping step 2-8 time;
(7) slurry stirred through (6) is continued under 40-70 DEG C of condition stirring to be concentrated in slurry containing TiO
2mass percent be 3-20%, obtain TiO
2slurry.
Further, described substrate refers to the slide of drying and processing again after washing powder rinsed clean, deionized water ultrasonic cleaning 3-7min.
Described strong magnetic agitation refers to that the magnetic apparatus with rotating speed is 300-600rpm stirs.
Nano-TiO in described step (1)
2the pure sharp titanium nano titanium oxide of powder to be particle diameter be 12-18nm.
Ethyl cellulose solution in described step (5) is under 40 DEG C of constant temperature stirring conditions, is slowly dissolved in by ethyl cellulose obtains in absolute ethyl alcohol according to the mass ratio of 1:12; Ethyoxyl mass content in described ethyl cellulose is 47.5%-49.0%.
Namely the present invention is with commercial titanium dioxide nano-powder for raw material and with absolute ethyl alcohol for dispersant, and using ethyl cellulose simultaneously as binding agent and pore creating material, is prepared into slurry, makes nano-TiO by progressively polishing
2granular composite is even, and makes the TiO that obtains
2slurry is not reunited, not stratified, dispersed, good stability.Then by spin-coating and high annealing method, by obtained TiO
2even, fine and close porous TiO prepared by slurry on substrate
2rete.
Relative to prior art, the present invention has following beneficial effect:
1, porous TiO of the present invention
2film adopts TiO
2slurry carries out prepared by spin-coating method, obtained film has even, the fine and close feature of film, and only containing two kinds of polymer substances in film, not only preparation process is easy, with low cost, and also easily removed the polymer substance contained in film by high annealing, thus 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, is then slowly scattered in absolute ethyl alcohol, then adds ethyl cellulose solution and terpinol wherein, the slurry prepared is not reunited, 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 relative to traditional slurry preparation process, the present invention only needs to add ethyl cellulose and these two kinds of polymer substances of 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.
Accompanying drawing explanation
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 are 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 are TiO
2electronic Speculum figure after film calcining;
Fig. 4 is TiO prepared by the embodiment of the present invention 2
2film is to the light degradation curve of 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 adopted in embodiment below
2powder selects particle diameter to be the pure sharp titanium nano titanium oxide of 15nm;
Strong magnetic agitation refers to that the magnetic apparatus with rotating speed is 300-600rpm stirs;
Selected ethyl cellulose solution is slowly dissolved in absolute ethyl alcohol according to the mass ratio of 1:12 by ethyl cellulose obtaining, and the ethyoxyl mass content wherein in ethyl cellulose is 47.5%-49.0%.
Embodiment 1:
(1) by nanometer 3gTiO
2powder and 3ml anhydrous acetic acid are put into ceramic mortar and are ground 8min;
(2) in (1), add 3ml deionized water and carry out grinding 6min, and repeat this operation 5 times;
(3) in (2), add 3ml absolute ethyl alcohol and carry out grinding 6min, and repeat this operation 15 times;
(4) in (3), add 6ml absolute ethyl alcohol and carry out grinding 6min, and repeat this operation 5 times;
(5) TiO that will obtain through (4) grinding
2slurry is transferred in beaker, under strong magnetic agitation, 1.5g ethyl cellulose solution and 0.9g terpinol is dropwise joined TiO successively
2in slurry, continue again after being added dropwise to complete to stir 1min;
(6) slurry obtained to (5) is left standstill 10s after ultrasonic process 10s in Ultrasound Instrument, then it is stirred 1min under strong magnetic agitation; Then repeat above-mentioned ultrasonic, leave standstill and whipping step 6 times;
(7) slurry stirred through (6) is continued under 50 DEG C of conditions stirring to be concentrated in slurry containing TiO
2mass percent be 20%, obtain TiO
2slurry.
(8) substrate: by slide drying and processing again after washing powder rinsed clean, deionized water ultrasonic cleaning 5min;
(9) glue machine is baked under the speed of 2000r/min by obtained TiO with even glue
2slurry for rotary coating on treated substrate, and at 60 DEG C drying and processing 1h;
(10) rete after oven dry is heat-treated to obtain porous TiO
2film, its heat treated annealing temperature is 420 DEG C, annealing time is 1 hour.
Porous TiO prepared by the present embodiment
2film amplifies the field emission scanning electron microscope figure of 2,000 times as shown in Figure 2, and the Electronic Speculum figure in Fig. 2 after d to be the Electronic Speculum figure before calcination, e be calcining, from figure, porous TiO prepared by the present invention
2film is very even, fine and close, and film after calcining still very evenly 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, the Electronic Speculum figure in Fig. 3 after f to be the Electronic Speculum figure before calcination, g be calcining, before and after its calcining, pattern of film is similar.
Embodiment 2:
(1) by nanometer 1.5gTiO
2powder and 3ml anhydrous acetic acid are put into ceramic mortar and are ground 3min;
(2) in (1), add 3ml deionized water and carry out grinding 2min, and repeat this operation 3 times;
(3) in (2), add 3ml absolute ethyl alcohol and carry out grinding 2min, and repeat this operation 10 times;
(4) in (3), add 6ml absolute ethyl alcohol and carry out grinding 5min, and repeat this operation 4 times;
(5) TiO that will obtain through (4) grinding
2slurry is transferred in beaker, under strong magnetic agitation, 1g ethyl cellulose solution and 1g terpinol is dropwise joined TiO successively
2in slurry, continue again after being added dropwise to complete to stir 2min;
(6) slurry obtained to (5) is left standstill 20s after ultrasonic process 20s in Ultrasound Instrument, then it is stirred 2min under strong magnetic agitation; Then repeat above-mentioned ultrasonic, leave standstill and whipping step 5 times;
(7) slurry stirred through (6) is continued under 45 DEG C of conditions stirring to be concentrated in slurry containing TiO
2mass percent be 15%, obtain TiO
2slurry.
(8) substrate: by slide drying and processing again after washing powder rinsed clean, deionized water ultrasonic cleaning 7min;
(9) glue machine is baked under the speed of 1800r/min by TiO with even glue
2slurry for rotary coating on substrate, and at 80 DEG C drying and processing 0.5h;
(10) rete after oven dry is heat-treated to obtain porous TiO
2film, its heat treated annealing temperature is 450 DEG C, annealing time is 1 hour.
Porous TiO prepared by the present embodiment
2film at calcination forward and backward light degradation curve h, i as shown in Figure 4 to methylene blue, the porous TiO obtained after 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 1gTiO
2powder and 1ml anhydrous acetic acid are put into ceramic mortar and are ground 2min;
(2) in (1), add 1ml deionized water and carry out grinding 2min, and repeat this operation 3 times;
(3) in (2), add 1ml absolute ethyl alcohol and carry out grinding 1min, and repeat this operation 8 times;
(4) in (3), add 2ml absolute ethyl alcohol and carry out grinding 1min, and repeat this operation 5 times;
(5) TiO that will obtain through (4) grinding
2slurry is transferred in beaker, under strong magnetic agitation, 0.5g ethyl cellulose solution and 0.5g terpinol is dropwise joined TiO successively
2in slurry, continue again after being added dropwise to complete to stir 1min;
(6) slurry obtained to (5) is left standstill 15s after ultrasonic process 15s in Ultrasound Instrument, then it is stirred 1min under strong magnetic agitation; Then repeat above-mentioned ultrasonic, leave standstill and whipping step 3 times;
(7) slurry stirred through (6) is continued under 50 DEG C of conditions stirring to be concentrated in slurry containing TiO
2mass percent be 10%, obtain TiO
2slurry.
(8) substrate; By slide drying and processing again after washing powder rinsed clean, deionized water ultrasonic cleaning 3min;
(9) glue machine is baked under the speed of 2500r/min by TiO with even glue
2slurry for rotary coating on substrate, and at 70 DEG C drying and processing 1h;
(10) rete after oven dry is heat-treated to obtain porous TiO
2film, its heat treated annealing temperature is 550 DEG C, annealing time is 0.8 hour.
Embodiment 4:
(1) by nanometer 2gTiO
2powder and 1ml anhydrous acetic acid are put into ceramic mortar and are ground 5min;
(2) in (1), add 2ml deionized water and carry out grinding 3min, and repeat this operation 7 times;
(3) in (2), add 2ml absolute ethyl alcohol and carry out grinding 2min, and repeat this operation 12 times;
(4) in (3), add 4ml absolute ethyl alcohol and carry out grinding 2min, and repeat this operation 8 times;
(5) TiO that will obtain through (4) grinding
2slurry is transferred in beaker, under strong magnetic agitation, 2g ethyl cellulose solution and 1.2g terpinol is dropwise joined TiO successively
2in slurry, continue again after being added dropwise to complete to stir 3min;
(6) slurry obtained to (5) is left standstill 25s after ultrasonic process 25s in Ultrasound Instrument, then it is stirred 1min under strong magnetic agitation; Then repeat above-mentioned ultrasonic, leave standstill and whipping step 6 times;
(7) slurry stirred through (6) is continued under 70 DEG C of conditions stirring to be concentrated in slurry containing TiO
2mass percent be 3%, obtain TiO
2slurry.
(8) substrate: by slide after washing powder rinsed clean, deionized water ultrasonic cleaning 5min again drying and processing obtain.
(9) glue machine is baked under the speed of 2000r/min by TiO with even glue
2slurry for rotary coating on substrate, and at 80 DEG C drying and processing 0.5h;
(10) rete after oven dry is heat-treated to obtain porous TiO
2film, its heat treated annealing temperature is 550 DEG C, annealing time is 0.5 hour.
Comparative example 1:
(1) by nanometer 1gTiO
2powder and 1ml anhydrous acetic acid are put into ceramic mortar and are ground 2min;
(2) in (1), add 1ml deionized water and carry out grinding 2min, and repeat this operation 3 times;
(3) in (2), add 1ml absolute ethyl alcohol and carry out grinding 1min, and repeat this operation 8 times;
(4) in (3), add 2ml absolute ethyl alcohol and carry out grinding 1min, and repeat this operation 5 times;
(5) TiO that will obtain through (4) grinding
2slurry is transferred in beaker, under strong magnetic agitation, 0.5g ethyl cellulose solution, 0.5g terpinol and 0.5g polyethylene glycol is joined TiO successively
2in slurry, continue again after being added dropwise to complete to stir 1min;
(6) slurry obtained to (5) is left standstill 15s after ultrasonic process 15s in Ultrasound Instrument, then it is stirred 1min under strong magnetic agitation; Then repeat above-mentioned ultrasonic, leave standstill and whipping step 3 times;
(7) slurry stirred through (6) is continued under 50 DEG C of conditions stirring to be concentrated in slurry containing TiO
2mass percent be 10%, obtain TiO
2slurry.
(8) substrate; By slide drying and processing again after washing powder rinsed clean, deionized water ultrasonic cleaning 3min;
(9) glue machine is baked under the speed of 2500r/min by TiO with even glue
2slurry for rotary coating on substrate, and at 70 DEG C drying and processing 1h.
Comparative example 2:
(1) P25 powder is carried out acid treatment before the test, adopt aqueous solution of nitric acid, controlling pH is at PH=2, and temperature processes 10 hours in the waters of 80 DEG C, processes later P25 dry for standby in the baking oven of 85 DEG C;
(2) take the P25 block 3g after acid treatment, mix with OP emulsifying agent, polyethylene glycol, water in mortar, the ratio of P25 block, OP emulsifying agent, PEG, water is 3:0.5:0.5:3, makes P25 block preliminarily solubilised;
(3) solution obtained 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 account for 15%, namely obtain titania slurry;
(5) substrate; By slide drying and processing again after washing powder rinsed clean, deionized water ultrasonic cleaning 3min;
(6) glue machine is baked under the speed of 2500r/min by TiO with even glue
2slurry for rotary coating on substrate, and at 70 DEG C drying and processing 1h.
Porous TiO prepared by embodiment 3
2the Electronic Speculum figure of film prepared by film and 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
2the film forming of slurry, uniformity and compactness all will be got well compared with the slurry of configuration in comparative example 1,2; And the present invention adds material only two kinds, this technology is simple, easy.
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: bake glue machine under the speed of 1800-2500r/min by TiO with even glue
2slurry for rotary coating on substrate, and at 60-80 DEG C drying and processing 0.5-1h; Then by dry after rete heat-treat, its heat treated annealing temperature is 420-550 DEG C, annealing time be 0.5-1 hour porous TiO
2film;
Described TiO
2slurry obtains 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
2be 1:0.5 ~ 2g/ml with the mass volume ratio of anhydrous acetic acid;
(2) in (1), add deionized water and carry out grinding 1-6min, and repeat this operation 3-10 time, described TiO
2be 1:0.5 ~ 2g/ml with the mass volume ratio of each addition of deionized water;
(3) in (2), add absolute ethyl alcohol and carry out grinding 1-6min, and repeat this operation 8-20 time, described TiO
2be 1:0.5 ~ 2g/ml with the mass volume ratio of each addition of absolute ethyl alcohol;
(4) in (3), add absolute ethyl alcohol and carry out grinding 1-6min, and repeat this operation 3-10 time, described TiO
2be 1:2 ~ 4g/ml with the mass volume ratio of each addition of absolute ethyl alcohol;
(5) TiO that will obtain through (4) grinding
2slurry is transferred in beaker, and under strong magnetic agitation, ethyl cellulose solution and terpinol is dropwise joined TiO successively
2in slurry, continue again after being added dropwise to complete 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 obtained to (5) is left standstill 10-30s after ultrasonic process 10-30s in Ultrasound Instrument, then it is stirred 1-5min under strong magnetic agitation; Then repeat above-mentioned ultrasonic, leave standstill and whipping step 2-8 time;
(7) slurry stirred through (6) is continued under 40-70 DEG C of condition stirring to be concentrated in slurry containing TiO
2mass percent be 3-20%, obtain TiO
2slurry.
2. porous TiO according to claim 1
2method for manufacturing thin film, is characterized in that: described substrate refers to the slide of drying and processing again after washing powder rinsed clean, deionized water ultrasonic cleaning 3-7min.
3. porous TiO according to claim 1
2method for manufacturing thin film, is characterized in that: described strong magnetic agitation refers to that the magnetic apparatus with rotating speed is 300-600rpm stirs.
4. porous TiO according to claim 1
2method for manufacturing thin film, is characterized in that: the nano-TiO in described step (1)
2the pure sharp titanium nano titanium oxide of powder to be particle diameter be 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, is slowly dissolved in by ethyl cellulose obtains 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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| CN102074374A (en) * | 2011-02-14 | 2011-05-25 | 合肥工业大学 | Doping dye sensitized solar cell photo anode, preparation method and application thereof |
| CN102332355A (en) * | 2011-04-13 | 2012-01-25 | 东旭集团有限公司 | Preparation technology for titanium dioxide nano membrane in dye-sensitized solar cell |
| CN103354177A (en) * | 2013-07-18 | 2013-10-16 | 南京大学昆山创新研究院 | TiO2 slurry used in large-area dye-sensitized solar cell preparation by screen printing technology and method for preparing the TiO2 slurry |
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| CN102074374A (en) * | 2011-02-14 | 2011-05-25 | 合肥工业大学 | Doping dye sensitized solar cell photo anode, preparation method and application thereof |
| CN102332355A (en) * | 2011-04-13 | 2012-01-25 | 东旭集团有限公司 | Preparation technology for titanium dioxide nano membrane in dye-sensitized solar cell |
| CN103354177A (en) * | 2013-07-18 | 2013-10-16 | 南京大学昆山创新研究院 | TiO2 slurry used in large-area dye-sensitized solar cell preparation by screen printing technology and method for preparing the TiO2 slurry |
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