CN106746713A - A kind of preparation method of titanium deoxid film self-cleaning glass - Google Patents
A kind of preparation method of titanium deoxid film self-cleaning glass Download PDFInfo
- Publication number
- CN106746713A CN106746713A CN201611105379.8A CN201611105379A CN106746713A CN 106746713 A CN106746713 A CN 106746713A CN 201611105379 A CN201611105379 A CN 201611105379A CN 106746713 A CN106746713 A CN 106746713A
- Authority
- CN
- China
- Prior art keywords
- preparation
- titanium deoxid
- cleaning glass
- glass
- deoxid film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/212—TiO2
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/71—Photocatalytic coatings
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/75—Hydrophilic and oleophilic coatings
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
Abstract
A kind of preparation method of titanium deoxid film self-cleaning glass, belongs to field of material preparation, it is characterised in that comprise the following steps：（1）Diethanol amine is added in absolute ethyl alcohol, acetic acid and distilled water stirring is added；（2）Butyl titanate is taken, is added dropwise in wherein, obtain TiO 2 sol；（3）Wash the greasy dirt of glass surface off with cleaning agent, soaked respectively with hydrochloric acid and NaOH after being rinsed with circulating water, the ion that may be remained on substrate is removed with distillation water washing, drying is made slide standby；（4）Slide is put into silicon dioxide gel, silicon dioxide gel discharge during using descent method, completes a coating process, multicoating repeated several times plated film after heat treatment completes glass preparation.Porous titanium dioxide thin-film self-cleaning glass is prepared using sol-gal process.There is optimal hydrophily and photocatalytic activity than self-cleaning glass film prepared by the improvement of, heat treatment temperature by coating layers, alcohol ester.
Description
Technical field
The invention belongs to field of material preparation, more particularly to a kind of preparation method of titanium deoxid film self-cleaning glass.
Background technology
Glass is the decorations in field such as orthodox car industry, building trade, modified stay material.With the hair of science and technology
Exhibition and the raising of human living standard, facing mankind increasingly severeer energy shortage, environmental pollution etc. are threatened and challenge, such as empty
Gas pollution can make glass article surface gradually in eclipse.In addition, after glass article surface has adsorbed the organic matter in air, shape
Into dirt, surface is dirty.The surface clean of glass has turned into the problem of daily life and maintenance, especially senior building curtain wall glass
There is work high above the ground in glass, its cleaning, dangerous big；There is certain corrosivity, while the waste water for producing brings secondary dirt to environment
Dye；Water consumption is big, wastes water resource.
Titanium dioxide is N-type semiconductor, when the photon irradiation of energy gap is more than by energy, will produce strong reducing property
Conduction band electron and strong oxidizing property valence band hole.Oxygen and moisture in active electronics and hole and local environment are made
With the photocatalytic for just generating titanium dioxide.Its catalytic oxidation performance decomposes each type organic, ultimately generate carbon dioxide and
Water, this process can make the organic matter on titanium deoxid film surface disappear.Again because titanium deoxid film is with hydrophilic well
Property, water droplet can wash away the inorganic matter of film surface.
The content of the invention
Present invention seek to address that above mentioned problem, there is provided a kind of preparation method of titanium deoxid film self-cleaning glass.
The technical scheme is that：
A kind of preparation method of titanium deoxid film self-cleaning glass, it is characterised in that comprise the following steps：
（1）8mL diethanol amine is added in 104mL absolute ethyl alcohols, in this, as inhibitor, delays the strong water of butyl titanate
Solution, adds acetic acid 20mL and distilled water 1mL, stirs 30-45min；
（2）Butyl titanate is taken, is added dropwise in wherein, stir 1h, be aged the TiO 2 sol stablized after 24h；
（3）Wash the greasy dirt of glass surface off with cleaning agent, then soaked respectively with hydrochloric acid and NaOH after being rinsed with circulating water
3h, then the ion that may be remained on substrate is removed with distillation water washing, the water of glass surface is dried up with hair-dryer finally, it is made
Slide is standby；
（4）Slide is put into silicon dioxide gel, silicon dioxide gel discharge during using descent method completes a plated film mistake
Journey, multicoating repeated several times plated film after heat treatment completes glass preparation.
The preparation method of titanium deoxid film self-cleaning glass of the present invention, the plating layer number is 3-5 layers.
The preparation method of titanium deoxid film self-cleaning glass of the present invention, the temperature of the heat treatment is 500-
550℃。
The preparation method of titanium deoxid film self-cleaning glass of the present invention, oh consumption is 10- to the butyl titanate
12mL。
The preparation method of titanium deoxid film self-cleaning glass of the present invention, the heat treatment is first dried at 80 DEG C
20min, is then transferred in Muffle furnace, after intensification is heat-treated, soaking time 2h.
The preparation method of titanium deoxid film self-cleaning glass of the present invention, the programming rate of the heat treatment process
It is 10 DEG C/min.
The technical effects of the invention are that：
The preparation method of titanium deoxid film self-cleaning glass of the present invention, butyl titanate is presoma, ethanol is solvent,
Diethanol amine is complexing agent, using second acid for adjusting pH, porous titanium dioxide thin-film self-cleaning glass is prepared using sol-gel process
Glass.There is optimal hydrophily than self-cleaning glass film prepared by the improvement of, heat treatment temperature by coating layers, alcohol ester
And photocatalytic activity.
Specific embodiment
Embodiment 1
A kind of preparation method of titanium deoxid film self-cleaning glass, it is characterised in that comprise the following steps：
（1）8mL diethanol amine is added in 104mL absolute ethyl alcohols, in this, as inhibitor, delays the strong water of butyl titanate
Solution, adds acetic acid 20mL and distilled water 1mL, stirs 30-45min；
（2）Butyl titanate is taken, is added dropwise in wherein, stir 1h, be aged the TiO 2 sol stablized after 24h；
（3）Wash the greasy dirt of glass surface off with cleaning agent, then soaked respectively with hydrochloric acid and NaOH after being rinsed with circulating water
3h, then the ion that may be remained on substrate is removed with distillation water washing, the water of glass surface is dried up with hair-dryer finally, it is made
Slide is standby；
（4）Slide is put into silicon dioxide gel, silicon dioxide gel discharge during using descent method completes a plated film mistake
Journey, multicoating repeated several times plated film after heat treatment completes glass preparation.
The preparation method of titanium deoxid film self-cleaning glass of the present invention, the plating layer number is 3 layers.
The preparation method of titanium deoxid film self-cleaning glass of the present invention, the temperature of the heat treatment is 500 DEG C.
The preparation method of titanium deoxid film self-cleaning glass of the present invention, oh consumption is the butyl titanate
10mL。
During coated glass inserted into methyl orange solution, using the h of 20 W ultra violet lamps 1, catalytic degradation methyl orange, then
Using Tv-1901 type ultraviolet-uisible spectrophotometers, the absorbance of the solution of methyl orange, plating is characterized with this after measure pre-irradiation
The photocatalysis performance of film.
Influence of the change of coating layers to film angle of wetting is little.The reason for causing this phenomenon is mainly due to film
Wettability is mainly influenceed by chemistry of solid surfaces composition, and Solid Surface Free Energy is bigger, easier by some liquid institutes
Wetting.In the preparation process of film, butyl titanate elder generation hydrolytic polymerization forms unbodied titanium deoxid film, then high temperature is moved back
Fire obtains the titanium deoxid film of anatase.By film thicker obtained from multiple plated film, its surface free energy is not sent out
Raw significant change, causes the contact angle on titanium deoxid film surface little with coating layers relation.
In the case where other conditions are not changed, when only changing the consumption of butyl titanate, the contact angle of glass is presented obvious
Change.The contact angle of glass is gradually reduced with the increase of the usage amount of butyl titanate within the specific limits, in butyl titanate
Consumption be 12 mL when reach minimum value.Then as the increase contact angle of the consumption of butyl titanate can become big again.This be due to
The titanium deoxid film prepared with sol-gel method is usually porous, with the increase of butyl titanate consumption, obtains
Microfine titanium dioxide particle increases, porosity increase, so angle of wetting reduces.But when butyl titanate consumption is excessive, can cause
Titanium dioxide granule is excessive, and porosity reduces, thus angle of wetting increase.
Embodiment 2
A kind of preparation method of titanium deoxid film self-cleaning glass, it is characterised in that comprise the following steps：
（1）8mL diethanol amine is added in 104mL absolute ethyl alcohols, in this, as inhibitor, delays the strong water of butyl titanate
Solution, adds acetic acid 20mL and distilled water 1mL, stirs 45min；
（2）Butyl titanate is taken, is added dropwise in wherein, stir 1h, be aged the TiO 2 sol stablized after 24h；
（3）Wash the greasy dirt of glass surface off with cleaning agent, then soaked respectively with hydrochloric acid and NaOH after being rinsed with circulating water
3h, then the ion that may be remained on substrate is removed with distillation water washing, the water of glass surface is dried up with hair-dryer finally, it is made
Slide is standby；
（4）Slide is put into silicon dioxide gel, silicon dioxide gel discharge during using descent method completes a plated film mistake
Journey, multicoating repeated several times plated film after heat treatment completes glass preparation.
The preparation method of titanium deoxid film self-cleaning glass of the present invention, the plating layer number is 5 layers.
The preparation method of titanium deoxid film self-cleaning glass of the present invention, the temperature of the heat treatment is 550 DEG C.
The preparation method of titanium deoxid film self-cleaning glass of the present invention, oh consumption is the butyl titanate
12mL。
The preparation method of titanium deoxid film self-cleaning glass of the present invention, the heat treatment is first dried at 80 DEG C
20min, is then transferred in Muffle furnace, after intensification is heat-treated, soaking time 2h.
The preparation method of titanium deoxid film self-cleaning glass of the present invention, the programming rate of the heat treatment process
It is 10 DEG C/min.
Contact angle influence of the heat treatment temperature on coated glass is very big, and this is mainly has with the crystal formation of TiO 2 coating film
Close.With the rising of temperature in the range of 400-500 DEG C, there is obvious reduction in contact angle, and subsequent contact angle tends to stabilization.
Temperature more than 550 DEG C after contact angle can become big again significantly depending on the rising of temperature, this is because film anatase is still at 400 DEG C
Do not formed completely, with respect to there is the relatively little of crystal face for producing Lacking oxygen for the 500 DEG C and 600 DEG C films for the treatment of, so
Contact angle is in the range of 400-500 DEG C as the rising of temperature is significantly reduced.Anatase is formed completely at 500 DEG C, institute
Stabilization is intended to the contact angle of glass and minimum value is reached, but a certain amount of titanium dioxide is changed into gold after 550 DEG C
Red stone, contact angle becomes big therewith again.
As coating layers increase to 5 from 3, the photocatalytic degradation capability of titanium deoxid film is significantly improved, after 5 layers
Resolution ratio is gradually reduced on the contrary.This is, because the increase of thickness causes film layer hole and catalysis active ingredient to increase, both to increase
The photochemical reaction area of film, improves the absorptivity of ultraviolet light again, and these factors cause degradation rate to improve.But if film is blocked up,
Surface titanium dioxide cohesion aggravation, the crystal grain increase in sintering process, effective TiO 2 particles surface area is just relative in film
Reduce, the utilization rate of light will be reduced, photocatalytic activity reduces.Film is thicker, and this influence is more serious.Optimal coating layers
It is 5 layers.
Photocatalytic activity influence of the heat treatment temperature on titanium deoxid film is very big.400 DEG C of sample catalysis activities for the treatment of
It is very poor.Temperature from rise to 500 DEG C for 400 DEG C when, with the rising of temperature, catalysis activity is significantly improved.500 DEG C for the treatment of
Sample photocatalytic activity highest, methyl orange degradation rate is up to 65%.When temperature is higher than 500 DEG C, with the rising dioxy of temperature
The photocatalytic activity for changing titanium film is substantially reduced, and it is anatase titanium dioxide crystalline phase stabilization that this is primarily due to 450-500 DEG C
The temperature of presence, its degraded to methyl orange shows photocatalytic activity very high under action of ultraviolet light.Calcining heat rises
For 550 DEG C when anatase can portions turn be rutile, form the mixed phase of the two, and the increase of rutile titanium dioxide is unfavorable
In the photocatalytic degradation of methyl orange.
Glass surface with optimum performance is integrally smooth, while again due to organic matter in heat treatment process
Volatilization, causes surface to be uniform-distribution with many small stomatas, and on the one hand this special surface texture advantageously reduces glass
Contact angle, on the one hand again can improve its photocatalysis performance.
Claims (6)
1. a kind of preparation method of titanium deoxid film self-cleaning glass, it is characterised in that comprise the following steps：
（1）8mL diethanol amine is added in 104mL absolute ethyl alcohols, in this, as inhibitor, delays the strong water of butyl titanate
Solution, adds acetic acid 20mL and distilled water 1mL, stirs 30-45min；
（2）Butyl titanate is taken, is added dropwise in wherein, stir 1h, be aged the TiO 2 sol stablized after 24h；
（3）Wash the greasy dirt of glass surface off with cleaning agent, then soaked respectively with hydrochloric acid and NaOH after being rinsed with circulating water
3h, then the ion that may be remained on substrate is removed with distillation water washing, the water of glass surface is dried up with hair-dryer finally, it is made
Slide is standby；
（4）Slide is put into silicon dioxide gel, silicon dioxide gel discharge during using descent method completes a plated film mistake
Journey, multicoating repeated several times plated film after heat treatment completes glass preparation.
2. the preparation method of titanium deoxid film self-cleaning glass according to claim 1, it is characterised in that：The coating
Quantity is 3-5 layers.
3. the preparation method of titanium deoxid film self-cleaning glass according to claim 1, it is characterised in that：At the heat
The temperature of reason is 500-550 DEG C.
4. the preparation method of titanium deoxid film self-cleaning glass according to claim 1, it is characterised in that：The metatitanic acid
Oh consumption is 10-12mL to butyl ester.
5. the preparation method of titanium deoxid film self-cleaning glass according to claim 1, it is characterised in that：At the heat
Reason first dries 20min at 80 DEG C, is then transferred in Muffle furnace, after intensification is heat-treated, soaking time 2h.
6. the preparation method of titanium deoxid film self-cleaning glass according to claim 5, it is characterised in that：At the heat
The programming rate of reason process is 10 DEG C/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611105379.8A CN106746713A (en) | 2016-12-05 | 2016-12-05 | A kind of preparation method of titanium deoxid film self-cleaning glass |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611105379.8A CN106746713A (en) | 2016-12-05 | 2016-12-05 | A kind of preparation method of titanium deoxid film self-cleaning glass |
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| CN106746713A true CN106746713A (en) | 2017-05-31 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111628120A (en) * | 2020-06-18 | 2020-09-04 | 苏州凌威新能源科技有限公司 | Lithium battery packaging film and preparation method thereof |
-
2016
- 2016-12-05 CN CN201611105379.8A patent/CN106746713A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111628120A (en) * | 2020-06-18 | 2020-09-04 | 苏州凌威新能源科技有限公司 | Lithium battery packaging film and preparation method thereof |
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170531 |
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| WD01 | Invention patent application deemed withdrawn after publication |