CN102515567A - Method for preparing nano CeO2 film having UV shielding property - Google Patents
Method for preparing nano CeO2 film having UV shielding property Download PDFInfo
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- CN102515567A CN102515567A CN201110415666XA CN201110415666A CN102515567A CN 102515567 A CN102515567 A CN 102515567A CN 201110415666X A CN201110415666X A CN 201110415666XA CN 201110415666 A CN201110415666 A CN 201110415666A CN 102515567 A CN102515567 A CN 102515567A
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Abstract
The invention relates to a method for preparing a nano CeO2 film having UV shielding property, comprising the following steps: adding a certain amount of cetyl trimethyl ammonium bromide (CTAB) in cyclohexane, and bringing to volume by cyclohexane to prepare a turbid CTAB-cyclohexane solution, adding the turbid CTAB-cyclohexane solution in a Ce(NO3)3.6H2O solution, adding isopropanol dropwisely to until the solution changes clear to obtain a microemulsion for painting a film; soaking a cleaned substrate into the microemulsion for painting films, painting the film by using a dip-coating method, and calcining to obtain the nano CeO2 film. The method has the advantages of simple process, easy operation, and few devices used herein, and the prepared film is continuous and uniform and has high transparency, and the prepared film can adsorb ultraviolet rays at 230-370 nm.
Description
Technical field
The present invention relates to a kind of nano Ce O with uv-shielding capacity
2The preparation method of film.
Background technology
In recent years, because the ozonosphere in the atmosphere is thin day by day, uitraviolet intensity increases, and strong excessively ultraviolet ray meeting damages the initiation various diseases to skin and the eyes of human body; In addition, ultraviolet ray can also make polymkeric substance degradation with agings such as resin, plastics, coating, rubber, the paper flavescence, becomes fragile, and it is extremely urgent therefore to develop various ultraviolet shielded materials.
Nano Ce O
2As a kind of novel rare earth functional materials, have the performance of many excellences and using value widely, received domestic and international researchist's common concern in recent years.At present, nano ceric oxide has been widely used in electronic ceramics, radioresistive glass, fuel cell, gas sensor, polishing material, and aspect such as cleaning catalyst for tail gases of automobiles.Nano Ce O
2Energy gap be 3.1eV, not only visible light is had perviousness preferably, and ultraviolet ray is had absorptive character preferably, be a kind of ultraviolet shielded material of wide spectrum, receive much concern.At present to CeO
2Powder research more, but,, be inconvenient to use as ultraviolet shielded material because powder is prone to reunite.
At present, preparation nano Ce O
2The method of film has pulse laser method, sol-gel method, chemical deposition etc.Pulse laser thin films cost is high, and the film that makes is thicker, and experimental installation complicacy, operation and control difficulty; The sol-gel thin films is consuming time longer, and experimentation is complicated; Chemical deposition prepares film, and film thickness is difficult to control, and it is inhomogeneous to form film.
Summary of the invention
Technical problem to be solved by this invention provides a kind of nano Ce O with uv-shielding capacity
2The preparation method of film, this method technology is simple, processing ease, equipment used is few, and the film that makes is continuous, even, transparency is high.
Technical solution of the present invention is:
A kind of nano Ce O with uv-shielding capacity
2The preparation method of film, its concrete steps are:
1, get a certain amount of cetyl trimethylammonium bromide (CTAB) and add in the hexanaphthene, and use the hexanaphthene constant volume, the muddy liquid of preparation CTAB-hexanaphthene, the content of CTAB is 0.7g/20mL～4.5g/20mL in the muddy liquid of described CTAB-hexanaphthene; It is joined the Ce (NO that concentration is 0.1mol/L～0.9mol/L
3)
36H
2In the O solution, muddy liquid of described CTAB-hexanaphthene and Ce (NO
3)
36H
2The volume ratio of O solution is 4:1; Drip Virahol to solution and clarify, must film and use microemulsion;
2, substrate is soaked 10min ~ 90min with sulfuric acid, take out the back washed with de-ionized water of using, 100 ℃ of following dry 1h ~ 4h, described substrate is sheet glass or quartz plate;
3, adopt dip-coating method to film; The substrate of cleaning is impregnated into the speed of 30mm/min～90mm/min films with in the microemulsion; Stop 20s～90s, to lift out with the identical speed of microemulsion with being impregnated into to film, at 80 ℃～120 ℃ times dry 5min～20min; Continuous impregnating lifts overlay film 1 time～8 times;
4, film substrate after finishing at 400 ℃～700 ℃ calcining 1h～5h down, be cooled to room temperature after, promptly make nano Ce O
2Film.
Above-mentioned nano Ce O with uv-shielding capacity
2The preparation method of film, the quality that contains CTAB in the muddy liquid of CTAB-hexanaphthene is 1.5g/20 mL～3.0g/20 mL.
Above-mentioned nano Ce O with uv-shielding capacity
2The preparation method of film, Ce (NO
3)
36H
2The concentration of O is 0.5mol/L～0.8mol/L.
Above-mentioned nano Ce O with uv-shielding capacity
2The preparation method of film, when filming, substrate is impregnated into to film and uses the speed in the microemulsion to be 30mm/min～60mm/min, and the residence time is 30s～60s in microemulsion.
Above-mentioned nano Ce O with uv-shielding capacity
2The preparation method of film, continuous impregnating lifts overlay film 1 time～5 times.
The present invention is with Ce (NO
3)
36H
2O is a water, and hexanaphthene is an oil phase, and cetyl trimethylammonium bromide (CTAB) is a tensio-active agent, and Virahol is a cosurfactant, stirs to make the clarification microemulsion; On substrate,, make nano Ce O after the calcining with the dip-coating method coated film
2Film.Whole technology is simple, processing ease, and equipment used is few, the CeO that makes
2Film is even continuously, and transparency is high, and the ultraviolet ray of 230nm～370nm is all had absorption.
Description of drawings
Fig. 1 is the nano Ce O that the present invention makes
2The SEM figure of film.
Embodiment
Embodiment 1
The CTAB that takes by weighing 4.37g is added in the hexanaphthene, and is settled to 20mL with hexanaphthene and gets the muddy liquid of CTAB-hexanaphthene; Getting 5mL concentration is the Ce (NO of 0.5mol/L
3)
36H
2O solution joins in the muddy liquid of 20mL CTAB-hexanaphthene of constant volume, and agitation condition drips Virahol to solution down and clarifies, and must film and use microemulsion; Quartz plate is soaked 10min with 80% sulfuric acid, take out the back washed with de-ionized water of using, 100 ℃ of following dry 1h; The washed glass sheet is impregnated into the speed of 60mm/min films with in the microemulsion, stop 90s after, lift out with the speed of 60mm/min, at 120 ℃ of dry 5min down; Calcine 2h down at 400 ℃, naturally cool to room temperature, obtain transparent film nano Ce O
2Film; Through ultraviolet-visible spectrophotometer detect film to ultraviolet absorption region at 240nm～360nm; Can find out by Fig. 1 and to make nano Ce O
2Thin film boundary is clear, explains that film is even continuously.
Embodiment 2
The CTAB that takes by weighing 0.73g is added in the hexanaphthene, and is settled to 20mL with hexanaphthene and gets the muddy liquid of CTAB-hexanaphthene; Getting 5mL concentration is the Ce (NO of 0.1 mol/L
3)
36H
2O solution joins in the muddy liquid of 20mL CTAB-hexanaphthene of constant volume, and agitation condition drips Virahol to solution down and clarifies, and must film and use microemulsion; Sheet glass is soaked 90 min with 50% sulfuric acid, take out the back washed with de-ionized water of using, 100 ℃ of following dry 1h; The washed glass sheet is impregnated into the speed of 90mm/min films with in the microemulsion, stop 20s after, lift out with the speed of 90mm/min, at 80 ℃ of dry 5min down, according to this operation, continuous impregnating lifts overlay film 8 times; Calcine 5h down at 400 ℃, naturally cool to room temperature, obtain transparent film nano Ce O
2Film; Through ultraviolet-visible spectrophotometer detect film to ultraviolet absorption region at 230nm～370nm.
Embodiment 3
The CTAB that takes by weighing 2.19g is added in the hexanaphthene, and is settled to 20mL with hexanaphthene and gets the muddy liquid of CTAB-hexanaphthene; Getting 5mL concentration is the Ce (NO of 0.8mol/L
3)
36H
2O solution joins in the muddy liquid of 20mL CTAB-hexanaphthene of constant volume, and agitation condition drips Virahol to solution down and clarifies, and must film and use microemulsion; Sheet glass is soaked 60 min with 50% sulfuric acid, take out the back washed with de-ionized water of using, 100 ℃ of following dry 2 h; The washed glass sheet is impregnated into the speed of 30mm/min films with in the microemulsion, stop 60s after, lift out with the speed of 30mm/min, at 90 ℃ of dry 10min down, according to this operation, continuous impregnating lifts overlay film 3 times; Calcine 3 h down at 500 ℃, naturally cool to room temperature, obtain transparent film nano Ce O
2Film; Through ultraviolet-visible spectrophotometer detect film to ultraviolet absorption region at 230nm～370nm.
Embodiment 4
The CTAB that takes by weighing 2.92g is added in the hexanaphthene, and is settled to 20mL with hexanaphthene and gets the muddy liquid of CTAB-hexanaphthene; Getting 5mL concentration is the Ce (NO of 0.3mol/L
3)
36H
2O solution joins in the muddy liquid of 20mL CTAB-hexanaphthene of constant volume, and agitation condition drips Virahol to solution down and clarifies, and must film and use microemulsion; Quartz plate is soaked 90 min with 30% sulfuric acid, take out the back washed with de-ionized water of using, 100 ℃ of following dry 3h; The washed glass sheet is impregnated into the speed of 60mm/min films with in the microemulsion, stop 20s after, lift out with the speed of 60mm/min, at 80 ℃ of dry 20min down, according to this operation, continuous impregnating lifts overlay film 2 times; Calcine 1h down at 700 ℃, naturally cool to room temperature, obtain transparent film nano Ce O
2Film; Through ultraviolet-visible spectrophotometer detect film to ultraviolet absorption region at 240nm～350nm.
Embodiment 5
The CTAB that takes by weighing 1.46g is added in the hexanaphthene, and is settled to 20mL with hexanaphthene and gets the muddy liquid of CTAB-hexanaphthene; Getting 5mL concentration is the Ce (NO of 0.9mol/L
3)
36H
2O solution joins in the muddy liquid of 20mLCTAB-hexanaphthene of constant volume, and agitation condition drips Virahol to solution down and clarifies, and must film and use microemulsion; Sheet glass is soaked 10 min with 98% sulfuric acid, take out the back washed with de-ionized water of using, 100 ℃ of following dry 2h; The washed glass sheet is impregnated into the speed of 45mm/min films with in the microemulsion, stop 40s after, lift out with the speed of 45mm/min, at 100 ℃ of dry 15min down, according to this operation, continuous impregnating lifts overlay film 5 times; Calcine 4h down at 600 ℃, naturally cool to room temperature, obtain transparent film nano Ce O
2Film; Through ultraviolet-visible spectrophotometer detect film to ultraviolet absorption region at 240nm～350nm.
Embodiment 6
The CTAB that takes by weighing 3.65g is added in the hexanaphthene, and is settled to 20mL with hexanaphthene and gets the muddy liquid of CTAB-hexanaphthene; Getting 5mL concentration is the Ce (NO of 0.6mol/L
3)
36H
2O solution joins in the muddy liquid of 20mLCTAB-hexanaphthene of constant volume, and agitation condition drips Virahol to solution down and clarifies, and must film and use microemulsion; Sheet glass is soaked 30min with 60% sulfuric acid, take out the back washed with de-ionized water of using, 100 ℃ of following dry 4h; The washed glass sheet is impregnated into the speed of 60mm/min films with in the microemulsion, stop 30s after, lift out with the speed of 60mm/min, at 110 ℃ of dry 5min down, according to this operation, continuous impregnating lifts overlay film 4 times; Calcine 2h down at 400 ℃, naturally cool to room temperature, obtain transparent film nano Ce O
2Film; Through ultraviolet-visible spectrophotometer detect film to ultraviolet absorption region at 240nm～370nm.
Claims (5)
1. nano Ce O with uv-shielding capacity
2The preparation method of film is characterized in that:
1.1 getting a certain amount of cetyl trimethylammonium bromide (CTAB) adds in the hexanaphthene; And use the hexanaphthene constant volume; The muddy liquid of preparation CTAB-hexanaphthene; The content of CTAB is 0.7g/20mL～4.5g/20mL in the muddy liquid of described CTAB-hexanaphthene, and it is joined the Ce (NO that concentration is 0.1mol/L～0.9mol/L
3)
36H
2In the O solution, muddy liquid of described CTAB-hexanaphthene and Ce (NO
3)
36H
2The volume ratio of O solution is 4:1; Drip Virahol to solution and clarify, must film and use microemulsion;
1.2 substrate is soaked 10min ~ 90min with sulfuric acid, take out the back washed with de-ionized water of using, 100 ℃ of following dry 1h ~ 4h, described substrate is sheet glass or quartz plate;
1.3 adopting dip-coating method films; The substrate of cleaning is impregnated into the speed of 30mm/min～90mm/min films with in the microemulsion; Stop 20s～90s, to lift out with the identical speed of microemulsion with being impregnated into to film, at 80 ℃～120 ℃ times dry 5min～20min; Continuous impregnating lifts overlay film 1 time～8 times;
Substrate after finishing 1.4 film is at 400 ℃～700 ℃ calcining 1h～5h down, be cooled to room temperature after, promptly make nano Ce O
2Film.
2. the nano Ce O with uv-shielding capacity according to claim 1
2The preparation method of film is characterized in that: the content of CTAB is 1.5g/20mL～3.0g/20mL in the muddy liquid of CTAB-hexanaphthene.
3. the nano Ce O with uv-shielding capacity according to claim 1
2The preparation method of film is characterized in that: Ce (NO
3)
36H
2The concentration of O is 0.5mol/L～0.8mol/L.
4. the nano Ce O with uv-shielding capacity according to claim 1
2The preparation method of film is characterized in that: when filming, substrate is impregnated into to film and uses the speed in the microemulsion to be 30mm/min～60mm/min, and the residence time is 30s～60s in microemulsion.
5. the nano Ce O with uv-shielding capacity according to claim 1
2The preparation method of film is characterized in that: continuous impregnating lifts overlay film 1 time～5 times.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110415666XA CN102515567A (en) | 2011-12-14 | 2011-12-14 | Method for preparing nano CeO2 film having UV shielding property |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110415666XA CN102515567A (en) | 2011-12-14 | 2011-12-14 | Method for preparing nano CeO2 film having UV shielding property |
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|---|---|
| CN102515567A true CN102515567A (en) | 2012-06-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105565373A (en) * | 2015-12-31 | 2016-05-11 | 包头稀土研究院 | Rare earth oxide-based nanometer ultraviolet shielding material and preparation method thereof |
Citations (6)
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|---|---|---|---|---|
| JP2000128580A (en) * | 1998-10-21 | 2000-05-09 | Toyota Motor Corp | Dip coating method for glass substrate |
| CN1400185A (en) * | 2001-07-31 | 2003-03-05 | 武汉理工大学 | Method for preparing high-activity titanium dioxide film self-cleaning glass material |
| CN101157522A (en) * | 2007-09-26 | 2008-04-09 | 武汉理工大学 | Visible light anti-reflection and ultraviolet radiation cut-off bifunctional coated glass and preparation method thereof |
| CN101538061A (en) * | 2009-05-06 | 2009-09-23 | 北京化工大学 | Method for preparing nano cerium dioxide |
| CN102060447A (en) * | 2010-11-26 | 2011-05-18 | 武汉理工大学 | Transparent coated glass with dual functions of preventing static electricity and cutting off ultraviolet rays and manufacturing method thereof |
| CN102115146A (en) * | 2011-01-06 | 2011-07-06 | 云南大学 | Nano-structured cerium oxide with and application thereof |
-
2011
- 2011-12-14 CN CN201110415666XA patent/CN102515567A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000128580A (en) * | 1998-10-21 | 2000-05-09 | Toyota Motor Corp | Dip coating method for glass substrate |
| CN1400185A (en) * | 2001-07-31 | 2003-03-05 | 武汉理工大学 | Method for preparing high-activity titanium dioxide film self-cleaning glass material |
| CN101157522A (en) * | 2007-09-26 | 2008-04-09 | 武汉理工大学 | Visible light anti-reflection and ultraviolet radiation cut-off bifunctional coated glass and preparation method thereof |
| CN101538061A (en) * | 2009-05-06 | 2009-09-23 | 北京化工大学 | Method for preparing nano cerium dioxide |
| CN102060447A (en) * | 2010-11-26 | 2011-05-18 | 武汉理工大学 | Transparent coated glass with dual functions of preventing static electricity and cutting off ultraviolet rays and manufacturing method thereof |
| CN102115146A (en) * | 2011-01-06 | 2011-07-06 | 云南大学 | Nano-structured cerium oxide with and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105565373A (en) * | 2015-12-31 | 2016-05-11 | 包头稀土研究院 | Rare earth oxide-based nanometer ultraviolet shielding material and preparation method thereof |
| CN105565373B (en) * | 2015-12-31 | 2017-04-26 | 包头稀土研究院 | Rare earth oxide-based nanometer ultraviolet shielding material and preparation method thereof |
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Application publication date: 20120627 |