CN106345449A - Oxidized-reduced graphene/TiO2:Nd composite self-cleaning film and preparation method thereof - Google Patents
Oxidized-reduced graphene/TiO2:Nd composite self-cleaning film and preparation method thereof Download PDFInfo
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- 238000004140 cleaning Methods 0.000 title claims abstract description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title abstract description 11
- 239000002131 composite material Substances 0.000 title abstract description 5
- 239000000243 solution Substances 0.000 claims abstract description 45
- 239000002243 precursor Substances 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 150000002500 ions Chemical class 0.000 claims abstract description 20
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- CFYGEIAZMVFFDE-UHFFFAOYSA-N neodymium(3+);trinitrate Chemical compound [Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CFYGEIAZMVFFDE-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 7
- 238000003618 dip coating Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 30
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 30
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 28
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 16
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 239000003381 stabilizer Substances 0.000 claims description 5
- 238000010304 firing Methods 0.000 abstract description 3
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004528 spin coating Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 33
- 239000010409 thin film Substances 0.000 description 27
- 230000001699 photocatalysis Effects 0.000 description 13
- 238000007146 photocatalysis Methods 0.000 description 12
- 239000000975 dye Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000003344 environmental pollutant Substances 0.000 description 5
- 231100000719 pollutant Toxicity 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- QBZIEGUIYWGBMY-FUZXWUMZSA-N (5Z)-5-hydroxyimino-6-oxonaphthalene-2-sulfonic acid iron Chemical compound [Fe].O\N=C1/C(=O)C=Cc2cc(ccc12)S(O)(=O)=O.O\N=C1/C(=O)C=Cc2cc(ccc12)S(O)(=O)=O.O\N=C1/C(=O)C=Cc2cc(ccc12)S(O)(=O)=O QBZIEGUIYWGBMY-FUZXWUMZSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- -1 graphite alkene Chemical class 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 229940002712 malachite green oxalate Drugs 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000000411 transmission spectrum Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Paints Or Removers (AREA)
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Abstract
The invention relates to an oxidized-reduced graphene/TiO2:Nd composite self-cleaning film and a preparation method thereof. The preparation method includes the steps of firstly, preparing a precursor solution, namely taking absolute ethyl alcohol and water as solvents, adding tetrabutyl titanate, neodymium nitrate and a GO aqueous solution into the solvents, and stirring sufficiently until a mixture is uniform and transparent so as to obtain the precursor solution, wherein the Ti ion concentration of the precursor solution is 0.01-0.10 mol/l, the Nd ion doping amount accounts for 0-1.5 at.% of TiO2, the mass ratio of oxidized-reduced graphene rGO to TiO2 is 0- 0.050 (0 is not included), water in the GO aqueous solution is counted into a total water proportion of the precursor solution, and 1.0 ml of concentrated hydrochloric acid is added into every 100 ml of precursor solution; secondly, coating, namely applying a substrate needing to be coated with the precursor solution by means of dip coating or spin coating, drying for 0.5 hour at 150-200 DEG C after every time of coating, and repeatedly coating for 5-25 times according to requirements; thirdly, firing for 1.0 hour at 400 DEG C so as to obtain the oxidized-reduced graphene/TiO2:Nd composite self-cleaning film on the substrate needing to be coated.
Description
Technical field
The present invention relates to self-cleaning film, specially oxidoreduction Graphene/tio2: nd complex self-cleaning film and its
Preparation method.
Background technology
Automatically cleaning is a critically important depollution of environment technology.Generally the thin film with self-cleaning performance is applied and carry out in interior
The surfaces such as External building thing, electrical equipment and armarium, play to the harmful gass in environment and the pollutant being attached to film surface
Photocatalysis Decomposition, sterilizing and reduce pollutant degree of adhesion effect, thus play environment purification etc. effect.Therefore, the world
There is extensive research and application various countries to self-cleaning film.
tio2Thin film due to have preferable photocatalysis and in the environment the performance such as stable be that the automatically cleaning commonly used at present is thin
Film.Self-cleaning film usually requires that there is good photocatalysis performance (pollutant of resolving harmful gas and attachment and going out
Bacterium), good electric conductivity (preventing the Electrostatic Absorption of pollutant), photo-induced super-hydrophilicity can (make some pollutant be difficult attached
And carried absorption water cleaning surface) and some apply (as glass pane) in necessary optical clarity energy.Although tio2Thin film has
There is preferable photocatalysis performance, but photocatalysis performance is still limited.By ion doping or/and with Graphene composite strengthening tio2
The photocatalysis performance of powder body material has extensive research and applies, and generally has more significant effect.But ion doping or/and
It is combined to tio with Graphene2The developmental research of film photocatalytic material seldom, and lacks that to have good conductive, photoinduction super close
Aqueouss and optical clarity energy ion doping tio2The exploitation of/graphene complex thin film.
Content of the invention
For problems of the prior art, the present invention provides a kind of oxidoreduction Graphene/tio2: nd complex is certainly
Cleaning film and preparation method thereof, this thin film has photocatalysis performance by force, conducts electricity very well, light is transparent, photoinduction is super hydrophilic
The excellent feature of property.
The present invention is to be achieved through the following technical solutions:
Oxidoreduction Graphene/tio2: nd complex self-cleaning film preparation method, comprise the steps,
Step 1, prepares precursor solution: with dehydrated alcohol and water as solvent, will be water-soluble to butyl titanate, neodymium nitrate and go
Liquid adds in solvent, obtains precursor solution through being stirred well to homogeneous transparent；Wherein, in precursor solution, ti ion concentration is
The doping of 0.01-0.10mol/l, nd ion is tio20-1.5at.%, oxidoreduction Graphene rgo and tio2Quality
Than for 0-0.050, and the content of the doping of nd ion and oxidoreduction Graphene rgo is not all 0；Water meter in go aqueous solution
Enter in total water proportioning of precursor solution, in every 100ml precursor solution, add 1.0ml concentrated hydrochloric acid；
Step 2, film: by precursor solution dip-coating or be spin-coated on the substrate needing plated film, in 150- after coating every time
0.5h is dried at 200 DEG C, repeatedly coats 5-25 time as requested；
Step 3, burns till: fire 1.0h at 400 DEG C, the substrate need plated film obtains oxidoreduction Graphene/
tio2: nd complex self-cleaning film.
Preferably, in step 1, the ethylene glycol, propylene glycol and the glycerol that add in a solvent are as stabilizer and dispersant.
Further, in step 1, wherein, the volume ratio of dehydrated alcohol, water, ethylene glycol, propylene glycol and glycerol is 3:1:2:
2:2.
Preferably, in step 1, in every 100ml precursor solution, add 5ml acetylacetone,2,4-pentanedione.
Preferably, described neodymium nitrate adopts six water neodymium nitrates.
Preferably, using magnetic force or ultrasonic be stirred well to homogeneous transparent during stirring.
Preferably, the concentration of go aqueous solution is 2mg/ml.
Oxidoreduction Graphene/tio2: nd complex self-cleaning film, it is obtained by preparation method of the present invention.
Compared with prior art, the present invention has a following beneficial technique effect:
The present invention passes through the trace rare-earth neodymium nd and composite graphite alkene rgo that adulterates, and is strengthened using the cooperative effect between two kinds
tio2Every self-cleaning performance of thin-film material；With pure smooth tio2Thin film, ion doping tio2Thin film and rgo/tio2Thin film phase
Ratio is hence it is evident that enhancing photocatalysis performance, electric conductivity and photo-induced super-hydrophilicity on the premise of optical clarity can affect very little
Energy.
Brief description
Fig. 1 a is the various nd/tio described in present example2Mol ratio and rgo/tio2Quality is urged in light than thin film
Change kinetic constant k that dye solution is during malachite green oxalate aqueous solution1Figure.
Fig. 1 b is the various nd/tio described in present example2Mol ratio and rgo/tio2Quality is urged in light than thin film
Change kinetic constant k that dye solution is during naphthol green b aqueous solution1Figure.
Fig. 2 is the photoconductive rate schematic diagram in present example.
Fig. 3 a is the various nd/tio described in present example2Mol ratio and rgo/tio2Quality is than thin film in ultraviolet
Infrared spectrogram before light irradiation.
Fig. 3 b is the various nd/tio described in present example2Mol ratio and rgo/tio2Quality is than thin film in ultraviolet
Infrared spectrogram after light irradiation.
Fig. 4 a is a part of nd/tio described in present example2Mol ratio and rgo/tio2Quality is than the light of thin film
Optical transmission spectra.
Fig. 4 b is another part nd/tio described in present example2Mol ratio and rgo/tio2Quality is than thin film
Light transmission rate spectrum.
Fig. 5 is the various nd/tio described in present example2Mol ratio and rgo/tio2Quality is than the resistance of thin film
Rate.
Fig. 6 is the rgo/tio described in present example2The xrd collection of illustrative plates of thin film when=0.05.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, described be explanation of the invention and
It is not to limit.
Example 1
Method for manufacturing thin film of the present invention is as follows.
1st, precursor solution preparation: solvent is dehydrated alcohol and water, stabilizer and dispersant are ethylene glycol, propylene glycol, third
Triol (glycerol)；Dehydrated alcohol, water, ethylene glycol, propylene glycol, the volume ratio of glycerol are 3:1:2:2:2.Every 100ml adds few
Amount concentrated hydrochloric acid 1.0ml plays the effect preventing hydroxide from being formed with redox graphene (go).Every 100ml adds 5ml second
Acyl acetone prevents tetrabutyl titanate hydrolysis.
Raw material: butyl titanate, neodymium nitrate (common for six water neodymium nitrates) and concentration are the go aqueous solution of 2mg/ml.Its
In, ti ion concentration is 0.01-0.10mol/l, too low film time long high cost, too high can reduce film performance.
In this preferred embodiment, based on 0.05mol/l, every 100ml solution adds butyl titanate 1.7016g to ti ion concentration.
Nd doping is tio20-1.5at.%, based on 0,0.5,1,1.5at.%, ti ion concentration presses 0.05mol/l
When, every 100ml precursor solution adds six water neodymium nitrate 0g, 0.0110g, 0.0219g and 0.0329g.
rgo/tio2Mass ratio is 0-0.050, by rgo/tio2Mass ratio=0.025 and 0.050 meter, ti ion concentration is pressed
During 0.05mol/l, every 100ml precursor solution adds go9.98mg (5mlgo aqueous solution) and 19.97mg respectively, and (10mlgo is water-soluble
Liquid).Water in go aqueous solution ought count in total water proportioning.Through magnetic force or ultrasonic be stirred well to homogeneous transparent.Obtain presoma
Solution.
2nd, film: glass etc. needs the substrate of plated film to be washed with detergent and EtOH Sonicate, applies dip coating or spin coating, often
After secondary painting, 150-200 DEG C is dried 0.5h, repeatedly applies 5-25 time as requested.
3rd, burn till: fire 1.0h at 400 DEG C and obtain oxidoreduction Graphene/tio2: nd complex self-cleaning film.
Oxidoreduction Graphene/tio of the present invention2: nd complex self-cleaning film, including optimum nd doping and rgo/
tio2Than.Adulterated tio by nd2/ rgo complex thin film, it has purer tio2Thin film, nd doping tio2Thin film and tio2/rgo
The preferable photocatalysis performance of complex thin film, as illustrated in figs. ia and ib；Increase rgo proportioning and nd content can increase photocatalysis and move
Mechanical constant k1, you can strengthen photocatalytic degradation capability.Wherein the dye solution of Fig. 1 a is malachite green oxalate aqueous solution, the dye of Fig. 1 b
Material solution is naphthol green b aqueous solution.k1By relational expressionThe slope of curve drawing is given；Wherein c0It is dyestuff with c
Concentration before solution photocatalysis and after photocatalysis t hour.
The present invention has preferable photoconductive performance, as shown in Fig. 2 increase rgo proportioning and nd content can increase film light
Conductivity.
The present invention has photo-induced super-hydrophilicity, if being less than 10 ° using the water contact angle of contact angle method test, difficulty has essence
True result.But can pass through thin film wave number in infrared spectrum is 3495cm-1And 1620cm-1Represent surface hydroxyl and absorption
The power of water absworption peak is strong and weak to weigh hydrophilic and photo-induced super-hydrophilicity.As shown in accompanying drawing 3a and Fig. 3 b, increase as seen from the figure
Big rgo proportioning and nd content can increase two absorption peak strength, you can increase hydrophilic and photo-induced super-hydrophilicity.
The present invention is in rgo/tio2≤ 0.05 and nd content is tio2≤ 1.5at% when can maintain tio2Film light is transparent
Performance does not have significant change, as shown in figures 4 a and 4b, although because film thickness difference result in a little transmitance differences, but light
Transmitance does not have the reduction of regularity with rgo proportioning and nd content, partly shows enhancing, rgo and nd is to light transmission for this explanation
The impact of rate is very little.
The present invention has preferable electric conductivity, as shown in figure 5, increase rgo proportioning and nd content are significantly reduced thin film
Resistivity, increase Thin film conductive rate.
Institute of the present invention made membrane is pure anatase phase, as shown in Figure 6.
The present invention passes through to control the content of nd mol ratio to increase to 1.5at% from 0, and every self-cleaning performance strengthens, can
It is applied to the occasion that properties all require.Wherein rgo/tio2Mass ratio increases to 0.05 from 0, and every self-cleaning performance increases
By force, it is applied to the occasion that properties all require.Strengthen more than 0.05 every self-cleaning performance but appearance color is more black, application
Can be occasion more black and that other properties require in appearance color.
The firing temperature of thin film of the present invention increases to 450 DEG C from 400 DEG C, and crystallite dimension increases, every self-cleaning performance
Weaken, therefore 400 DEG C is rational firing temperature.
Example 2
Oxidoreduction Graphene/tio2: nd complex self-cleaning film preparation method, comprise the steps,
Step 1, prepares precursor solution: with dehydrated alcohol and water as solvent, will be water-soluble to butyl titanate, neodymium nitrate and go
Liquid adds in solvent, obtains precursor solution using magnetic force or the ultrasonic homogeneous transparent that is stirred well to；Wherein, in precursor solution
Ti ion concentration is 0.01mol/l, and the doping of nd ion is tio20.1at.%, oxidoreduction Graphene rgo and tio2's
Mass ratio is 0.010；Water in go aqueous solution counts in total water proportioning of precursor solution, adds in every 100ml precursor solution
Enter 1.0ml concentrated hydrochloric acid；The concentration of go aqueous solution is 2mg/ml, and neodymium nitrate adopts six water neodymium nitrates.
Step 2, film: by precursor solution dip-coating or be spin-coated on the substrate needing plated film, at 150 DEG C after coating every time
Under 0.5h is dried, repeatedly coat 5 times；
Step 3, burns till: fire 1.0h at 400 DEG C, the substrate need plated film obtains oxidoreduction Graphene/
tio2: nd complex self-cleaning film.
The ethylene glycol, propylene glycol and the glycerol that add in a solvent are as stabilizer and dispersant；Dehydrated alcohol, water, second
The volume ratio of glycol, propylene glycol and glycerol is 3:1:2:2:2.5ml acetylacetone,2,4-pentanedione is added in every 100ml precursor solution.
Example 3
Oxidoreduction Graphene/tio2: nd complex self-cleaning film preparation method, comprise the steps,
Step 1, prepares precursor solution: with dehydrated alcohol and water as solvent, will be water-soluble to butyl titanate, neodymium nitrate and go
Liquid adds in solvent, obtains precursor solution using magnetic force or the ultrasonic homogeneous transparent that is stirred well to；Wherein, in precursor solution
Ti ion concentration is 0.10mol/l, and the doping of nd ion is tio21.5at.%, oxidoreduction Graphene rgo and tio2's
Mass ratio is 0.050；Water in go aqueous solution counts in total water proportioning of precursor solution, adds in every 100ml precursor solution
Enter 1.0ml concentrated hydrochloric acid；The concentration of go aqueous solution is 2mg/ml, and neodymium nitrate adopts six water neodymium nitrates.
Step 2, film: by precursor solution dip-coating or be spin-coated on the substrate needing plated film, at 200 DEG C after coating every time
Under 0.5h is dried, repeatedly coat 25 times；
Step 3, burns till: fire 1.0h at 400 DEG C, the substrate need plated film obtains oxidoreduction Graphene/
tio2: nd complex self-cleaning film.
The ethylene glycol, propylene glycol and the glycerol that add in a solvent are as stabilizer and dispersant；Dehydrated alcohol, water, second
The volume ratio of glycol, propylene glycol and glycerol is 3:1:2:2:2.5ml acetylacetone,2,4-pentanedione is added in every 100ml precursor solution.
Claims (8)
1. oxidoreduction Graphene/tio2: nd complex self-cleaning film preparation method it is characterised in that comprising the steps,
Step 1, prepares precursor solution: with dehydrated alcohol and water as solvent, butyl titanate, neodymium nitrate and go aqueous solution is added
Enter in solvent, obtain precursor solution through being stirred well to homogeneous transparent；Wherein, in precursor solution, ti ion concentration is
The doping of 0.01-0.10mol/l, nd ion is tio20-1.5at.%, oxidoreduction Graphene rgo and tio2Quality
Than for 0-0.050, and the content of the doping of nd ion and oxidoreduction Graphene rgo is not all 0；Water meter in go aqueous solution
Enter in total water proportioning of precursor solution, in every 100ml precursor solution, add 1.0ml concentrated hydrochloric acid；
Step 2, film: by precursor solution dip-coating or be spin-coated on the substrate needing plated film, at 150-200 DEG C after coating every time
Under 0.5h is dried, as requested repeatedly coat 5-25 time；
Step 3, burns till: fires 1.0h at 400 DEG C, obtains oxidoreduction Graphene/tio on the substrate need plated film2: nd
Complex self-cleaning film.
2. oxidoreduction Graphene/tio according to claim 12: nd complex self-cleaning film preparation method, its feature
It is, in step 1, the ethylene glycol, propylene glycol and the glycerol that add in a solvent are as stabilizer and dispersant.
3. oxidoreduction Graphene/tio according to claim 22: nd complex self-cleaning film preparation method, its feature
It is, in step 1, wherein, the volume ratio of dehydrated alcohol, water, ethylene glycol, propylene glycol and glycerol is 3:1:2:2:2.
4. oxidoreduction Graphene/tio according to claim 12: nd complex self-cleaning film preparation method, its feature
It is, in step 1, in every 100ml precursor solution, add 5ml acetylacetone,2,4-pentanedione.
5. oxidoreduction Graphene/tio according to claim 12: nd complex self-cleaning film preparation method, its feature
It is, described neodymium nitrate adopts six water neodymium nitrates.
6. oxidoreduction Graphene/tio according to claim 12: nd complex self-cleaning film preparation method, its feature
It is, using magnetic force or ultrasonic be stirred well to homogeneous transparent during stirring.
7. oxidoreduction Graphene/tio according to claim 12: nd complex self-cleaning film preparation method, its feature
It is, the concentration of go aqueous solution is 2mg/ml.
8. oxidoreduction Graphene/tio2: nd complex self-cleaning film is it is characterised in that by any one in claim 1-7
Preparation method described in is obtained.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1669934A (en) * | 2005-03-04 | 2005-09-21 | 河北工业大学 | Tourmaline/titanium dioxide composite collosol containing rare earth and its preparation method and uses |
| CN102631910A (en) * | 2012-03-20 | 2012-08-15 | 中国海洋石油总公司 | Stable graphene/titanium oxide composite nanosol and preparation method thereof |
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| CN1669934A (en) * | 2005-03-04 | 2005-09-21 | 河北工业大学 | Tourmaline/titanium dioxide composite collosol containing rare earth and its preparation method and uses |
| CN102631910A (en) * | 2012-03-20 | 2012-08-15 | 中国海洋石油总公司 | Stable graphene/titanium oxide composite nanosol and preparation method thereof |
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